A kind of method that hydroxylamine sulfate and calcium oxide prepare caprylyl hydroxamic acid

A technology of hydroxylamine sulfate and caprylyl hydroxamic acid, which is applied in the direction of organic chemistry, can solve the problems of lack of effective methods for acylhydroxamic acid solids, and achieve the effects of efficient preparation, reduced production costs, and convenient operation of the method

Active Publication Date: 2020-11-10
禹城禹圳生物科技有限公司
View PDF10 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In summary, there is still a lack of effective methods for the preparation of acylhydroxamic acid solids from hydroxylamine sulfate

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] At 0-10°C, add 16.8g of quicklime (0.3mol) in batches into a reaction flask containing 49.2g of hydroxylamine sulfate (0.3mol) and 200g of methanol, keep the inner temperature below 10°C, and wait until the quicklime is added , continue to react for 30 minutes, filter to remove calcium sulfate solid, add 16.8g quicklime (0.3mol) and 79g methyl octanoate (0.5mol) to the filtrate successively, then raise the temperature to 50°C, react for 2 hours, and remove by vacuum distillation Methanol solvent, then add 400g water, lower the temperature to 0°C, control the internal temperature not to exceed 10°C, adjust the pH value of the system to 3-4 with 10% hydrochloric acid, and precipitate a white solid of octanoylhydroxamic acid, filter, wash with water, and dry. 63.8 g (yield 80.3%) of octanoyl hydroxamic acid was obtained, 1 H NMR (DMSO‐d6, 400MHz): δ10.33(br,1H), 8.64(br,1H), 1.92(t,2H), 1.54‐1.41(m,2H), 1.34‐1.15(m,8H) ,0.86(t,3H).

Embodiment 2

[0026] At 0-10°C, add 16.8g of quicklime (0.3mol) in batches into a reaction flask containing 49.2g of hydroxylamine sulfate (0.3mol) and 200g of methanol, keep the inner temperature below 10°C, and wait until the quicklime is added , continue to react for 30 minutes, filter to remove calcium sulfate solid, add 16.8g quicklime (0.3mol) and 79g methyl octanoate (0.5mol) to the filtrate successively, then raise the temperature to 60°C, react for 2 hours, and remove by vacuum distillation Methanol solvent, then add 400g water, lower the temperature to 0°C, control the internal temperature not to exceed 10°C, adjust the pH value of the system to 3-4 with 10% hydrochloric acid, and precipitate a white solid of octanoylhydroxamic acid, filter, wash with water, and dry. 63.4 g of octanoylhydroxamic acid was obtained (yield 79.7%).

Embodiment 3

[0028] At 0-10°C, add 16.8g of quicklime (0.3mol) in batches into a reaction flask containing 49.2g of hydroxylamine sulfate (0.3mol) and 200g of methanol, keep the inner temperature below 10°C, and wait until the quicklime is added , continue to react for 30 minutes, filter to remove calcium sulfate solid, add 16.8g quicklime (0.3mol) and 79g methyl octanoate (0.5mol) to the filtrate successively, then raise the temperature to 40°C, react for 2 hours, and remove by vacuum distillation Methanol solvent, then add 400g water, lower the temperature to 0°C, control the internal temperature not to exceed 10°C, adjust the pH value of the system to 3-4 with 10% hydrochloric acid, and precipitate a white solid of octanoylhydroxamic acid, filter, wash with water, and dry. 57.3 g of octanoylhydroxamic acid was obtained (yield 72.1%).

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention relates to a method for preparing octanohydroxamic acid from hydroxylamine sulfate and calcium oxide and belongs to the field of cosmetic raw material synthesis. The method is characterized by comprising the following steps of adding quicklime into a hydroxylamine sulfate solution at a temperature of less than or equal to 10 DEG C, filtering away precipitated calcium sulfate, sequentially adding the quicklime and methyl caprylate, performing hydroxyl oximation reaction at 30-60 DEG C, recovering a solvent after 2-6h, cooling to 0 DEG C, adding 10% hydrochloric acid at the low temperature, regulating a pH (potential of hydrogen) value to 3-4, precipitating octanohydroxamic acid solid, performing filtering, water washing and dryness to form octanohydroxamic acid. The method is mild in reaction condition and high in yield; a product is good in purity; the cheap and readily accessible quicklime is used as alkali, so that the raw material cost is greatly lowered; and the method is applicable to industrial production.

Description

technical field [0001] The invention relates to a method for preparing octanoylhydroxamic acid from hydroxylamine sulfate and calcium oxide, and belongs to the field of cosmetic raw material synthesis. Background technique [0002] The existing production process mainly uses hydroxylamine hydrochloride as the source of hydroxylamine, but there are also a small number of documents using hydroxylamine sulfate as a substitute. [0003] In the 1970s, Shchukina introduced a process (Khim.Prom., Moscow, 1970, 49 (3), 220) for the preparation of acylhydroxamic acid from hydroxylamine sulfate. In this method, methyl carboxylate, hydroxylamine sulfate and The mixed system of sodium hydroxide is first reacted at 20-25°C for 2 hours, then heated to 55-60°C for 1 hour, and then acidified to pH 4-5 at a temperature lower than 40°C to obtain free C7- 9 Acylohydroxamic acid with a yield of 72-78%. [0004] On this basis, the Russian patent (USSR Pat.390074, 1973-7-11) used 3 to 5% anioni...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): C07C259/06
CPCC07C259/06
Inventor 赵景瑞焦志刚杨正龙邹忠华翟宏斌
Owner 禹城禹圳生物科技有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap