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Reduced pressure distillation device and method for preparing N-methyl-2-chloroethyl pyrrolidine

A technology for producing and distilling chloroethylpyrrolidine, which is applied in vacuum distillation, distillation regulation/control, organic chemistry, etc., can solve problems such as low distillation efficiency and unfavorable steam, achieve high distillation efficiency, realize condensation, and increase speed Effect

Inactive Publication Date: 2021-12-24
赵美芳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The preparation process of N-methyl-2-chloroethylpyrrolidine needs to be purified by vacuum distillation, but the existing vacuum distillation device is that the raw material is heated from bottom to top, which is not conducive to the rapid generation of steam at the top of the material. makes the overall distillation efficiency low

Method used

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  • Reduced pressure distillation device and method for preparing N-methyl-2-chloroethyl pyrrolidine
  • Reduced pressure distillation device and method for preparing N-methyl-2-chloroethyl pyrrolidine
  • Reduced pressure distillation device and method for preparing N-methyl-2-chloroethyl pyrrolidine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Such as figure 1 , 2, a kind of N-methyl-2-chloroethylpyrrolidine preparation shown in 3, 4, 5, 8, and 9 uses a vacuum distillation device, including a distillation tank 1, a sewage pipe 3, a feed pipe 4, and a collection tank 12 and a cover plate 14, the observation tube 2 is fixedly installed in the mounting hole at the upper end of the side wall of the retort 1, the bottom of the side wall of the retort 1 is fixedly connected with a blowdown pipe 3, the retort 1 is connected with a cover plate 14, and the cover plate 14 The side wall is fixedly connected with the feed pipe 4, and the side wall of the cover plate 14 is fixedly installed with a temperature sensor 5 for temperature monitoring. The top of the cover plate 14 is connected with a constant temperature stirring structure for constant temperature stirring of the solution. The constant temperature stirring structure includes a drive Motor 6, hot air inlet pipe 7, electric heater fan 15, hot air outlet pipe 16,...

Embodiment 2

[0043] Embodiment 2 is a further improvement to Embodiment 1.

[0044] Such as image 3 , 4 , 7, the driving structure includes the fan blade 24, the first ring gear 25, the L-shaped mounting plate 26, the second ring gear 27 and the rotating shaft 31, the first ring gear 25 is fixedly installed on the outer wall of the hollow rotating shaft 20, the first tooth The ring 25 is evenly meshed with the second ring gear 27 along the circumferential direction, and the middle end straight hole of the second ring gear 27 is fixedly connected with the rotating shaft 31, and the top of the rotating shaft 31 is uniformly fixedly connected with the fan blade 24 along the circumferential direction. The lateral portion of the L-shaped mounting plate 26 is rotatably connected to the rotating shaft 31 through a fixedly connected bearing, and the L-shaped mounting plate 26 is fixedly mounted on the inner wall of the cover plate 14, and the hollow rotating shaft 20 drives the first ring gear 2...

Embodiment 3

[0046] Embodiment 3 is a further improvement to Embodiment 1.

[0047] Such as figure 1 , 3 , 4, 5, and 6, the cycle condensation structure includes steam outlet pipe 8, condensation pipe 9, cold water inlet pipe 10, straight pipe 11, steam inlet pipe 13, water outlet pipe 17, vortex capillary tube 22 and connecting pipe 23, steam The outlet pipe 8 is fixedly installed on the side wall of the cover plate 14, and the bottom of the outer end of the steam outlet pipe 8 is fixedly connected with a condensing pipe 9, and the side wall of the condensing pipe 9 is evenly and fixedly connected with a connecting pipe 23, and the outer end of the connecting pipe 23 is fixedly connected A cold water inlet pipe 10 is arranged, and the cold water inlet pipe 10 is connected with a cold water source. The inner end of the connecting pipe 23 is fixedly connected with a vortex capillary 22, and the inner end of the vortex capillary 22 is fixedly connected with the outer end of the water outlet...

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Abstract

The invention discloses a reduced pressure distillation device and method for preparing N-methyl-2-chloroethyl pyrrolidine, and relates to the field of pyrrolidine synthesis. The reduced pressure distillation device comprises a distillation retort, a blow-off pipe, a feeding pipe, a collecting tank and a cover plate, the blow-off pipe is fixedly connected to the bottom of the side wall of the distillation retort, the distillation retort is connected with the cover plate, the feeding pipe is fixedly connected to the side wall of the cover plate, a temperature sensor used for temperature monitoring is fixedly installed on the side wall of the cover plate, the top of the cover plate is connected with a constant-temperature stirring structure used for constant-temperature stirring of a solution, the constant-temperature stirring structure is connected with a driving structure used for driving gas to flow, and the cover plate is connected with a circulating condensation structure used for circulating condensation. The bottom of the circulating condensation structure is movably and hermetically connected with a collecting tank for collecting N-methyl-observation tube-chloroethyl pyrrolidine; the temperature of raw materials in the distillation retort is ensured to be in a balanced state, upper and lower layer temperatures of the raw materials are prevented from being unbalanced, steam can be quickly generated at the top of the materials, and the whole distillation efficiency is high.

Description

technical field [0001] The invention relates to the field of pyrrolidine synthesis, in particular to a vacuum distillation device and method for preparing N-methyl-2-chloroethyl pyrrolidine. Background technique [0002] N-methyl-2-chloroethylpyrrolidine is the raw material for the preparation of (S)-N-methyl-2-chloroethylpyrrolidine, and (S)-N-methyl-2-chloroethylpyrrolidine It is an important intermediate for the preparation of antihistamine clemastine fumarate. Clemastine Fumarate is an antihistamine successfully developed by the Swiss company Sandoz in the 1960s. As a representative second-generation H1 receptor antagonist, it is clinically used for the treatment of Histamine has caused various allergic diseases, and it is currently recognized as one of the best antihistamines in the world. [0003] The preparation process of N-methyl-2-chloroethylpyrrolidine needs to be purified by vacuum distillation, but the existing vacuum distillation device is that the raw materi...

Claims

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Application Information

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IPC IPC(8): B01D3/10B01D3/42C07D207/08
CPCB01D3/10B01D3/42C07D207/08
Inventor 赵美芳
Owner 赵美芳
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