Method for synthesizing high-precision allyl carboxylate by Schlecker pipe

An allyl carboxylate, high-precision technology, which is applied in the preparation of carboxylate esters, chemical instruments and methods, and the preparation of organic compounds, and can solve problems such as poor precision, environmental protection, and complicated processes

Inactive Publication Date: 2018-11-02
程桂平
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In the prior art, the method for synthesizing high-precision allyl carboxylate using Schleck tubes is complicated, has poor precision, and is not environmentally friendly.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A kind of method utilizing Schleck tube to synthesize high-precision allyl carboxylate, comprising:

[0022] Step 1: Take a dry 25mL Schleck tube;

[0023] Step 2: the dicyclopentadienyl zirconium dichloride weighing 29.2mg joins in the Schlack tube;

[0024] Step 3: Connect the Schleck tube to the double row tube;

[0025] Step 4: evacuate the oil pump for half an hour at 50°C;

[0026] Step 5: Then replace the air with nitrogen 5 times;

[0027] Step 6: Add 2.1 mg of zirconocene hydrochloride, and add 2 ml of dimethyl terephthalate that is strictly dehydrated;

[0028] Step 7: Add 2mL of 1,4-epoxybutane through strict water removal;

[0029] Step 8: Cool the reaction system to -78°C with a liquid nitrogen acetone bath;

[0030] Step 9: Add 1.1 mL of ethylmagnesium chloride dropwise under nitrogen protection, and then add 1 mmol of monosubstituted alkene;

[0031] Step 10: react at -78 ° C for 1 h, remove the liquid nitrogen acetone bath, naturally rise to room t...

Embodiment 2

[0038] A kind of method utilizing Schleck tube to synthesize high-precision allyl carboxylate, comprising:

[0039] Step 1: Take a dry 25mL Schleck tube;

[0040] Step 2: the dicyclopentadienyl zirconium dichloride weighing 29.2mg joins in the Schlack tube;

[0041] Step 3: Connect the Schleck tube to the double row tube;

[0042] Step 4: evacuate the oil pump for half an hour at 50°C;

[0043] Step 5: Then replace the air with nitrogen 5 times;

[0044] Step 6: Add 2.2 mg of zirconocene hydrochloride, and add 2 ml of dimethyl terephthalate that is strictly dehydrated;

[0045] Step 7: Add 2mL of 1,4-epoxybutane through strict water removal;

[0046] Step 8: Cool the reaction system to -78°C with a liquid nitrogen acetone bath;

[0047] Step 9: Add 1.1 mL of ethylmagnesium chloride dropwise under nitrogen protection, and then add 1 mmol of monosubstituted alkene;

[0048] Step 10: react at -78 ° C for 1 h, remove the liquid nitrogen acetone bath, naturally rise to room t...

Embodiment 3

[0055] A kind of method utilizing Schleck tube to synthesize high-precision allyl carboxylate, comprising:

[0056] Step 1: Take a dry 25mL Schleck tube;

[0057] Step 2: the dicyclopentadienyl zirconium dichloride weighing 29.2mg joins in the Schlack tube;

[0058] Step 3: Connect the Schleck tube to the double row tube;

[0059] Step 4: evacuate the oil pump for half an hour at 50°C;

[0060] Step 5: Then replace the air with nitrogen 5 times;

[0061] Step 6: add 2.3 mg of zirconocene hydrochloride, and add 2 ml of dimethyl terephthalate that is strictly dehydrated;

[0062] Step 7: Add 2mL of 1,4-epoxybutane through strict water removal;

[0063] Step 8: Cool the reaction system to -78°C with a liquid nitrogen acetone bath;

[0064] Step 9: Add 1.1 mL of ethylmagnesium chloride dropwise under nitrogen protection, and then add 1 mmol of monosubstituted alkene;

[0065] Step 10: react at -78 ° C for 1 h, remove the liquid nitrogen acetone bath, naturally rise to room t...

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PUM

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Abstract

The invention provides a method for synthesizing high-precision allyl carboxylate by a Schlecker pipe. The method comprises the following steps of taking a dry 25mL Schlecker pipe; 2, weighing 29.2mgof bicyclopentadienylidene zirconium dichloride into the Schlecker pipe; 3, connecting the Schlecker pipe onto a double-row pipe.

Description

technical field [0001] The invention relates to a method for synthesizing high-precision allyl carboxylate by utilizing a Schleck tube. Background technique [0002] In the prior art, the method for synthesizing high-precision allyl carboxylate using Schleck tubes is complicated, has poor precision, and is not environmentally friendly. Contents of the invention [0003] A kind of method utilizing Schleck tube to synthesize high-precision allyl carboxylate, comprising: [0004] Step 1: Take a dry 25mL Schleck tube; [0005] Step 2: the dicyclopentadienyl zirconium dichloride weighing 29.2mg joins in the Schlack tube; [0006] Step 3: Connect the Schleck tube to the double row tube; [0007] Step 4: evacuate the oil pump for half an hour at 50°C; [0008] Step 5: Then replace the air with nitrogen 5 times; [0009] Step 6: Add 2.1 mg of zirconocene hydrochloride, and add 2 ml of dimethyl terephthalate that is strictly dehydrated; [0010] Step 7: Add 2mL of 1,4-epoxybu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/00C07C69/83
CPCC07C67/00C07C69/82
Inventor 程桂平
Owner 程桂平
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