Method for preparing diethylamino hydroxybenzoyl hexyl benzoate

A technology of diethylamino hydroxybenzoyl benzoic acid and hydroxybenzoyl, which is applied in the field of manufacturing diethylamino hydroxybenzoyl hexyl benzoate, can solve problems such as difficulty in application and mass production constraints, and achieve mass production Effects of production, high yield, and reduced number of purifications

Pending Publication Date: 2022-01-28
AS科技有限公司
View PDF2 Cites 1 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crystallization method disclosed in said patent is a method of obtaining DHHB in a solid form by recooling to a temperature lower than the melting point after complete dissolution at a temperat...

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing diethylamino hydroxybenzoyl hexyl benzoate
  • Method for preparing diethylamino hydroxybenzoyl hexyl benzoate
  • Method for preparing diethylamino hydroxybenzoyl hexyl benzoate

Examples

Experimental program
Comparison scheme
Effect test

manufacture example 1

[0061] Production Example 1. Synthesis of 2-(4-N,N-diethylamino-2-hydroxybenzoyl)benzoic acid

[0062] After putting 3-diethylaminophenol (1.0 kg, 7.87 mol) and phthalic anhydride (1.17 kg, 7.87 mol) into the 3-neck flask, it was stirred with toluene (5.0 L). After raising the internal temperature of the reactor to 110-115° C. and stirring for 2 hours, it was cooled to 0-10° C. and the precipitated solid was filtered to obtain the title compound (1.7 kg, 89.9%).

[0063] 1 H NMR (CDCl 3 ): 12.52(s,1H),7.91(dd,1H),7.62(m,2H),7.33(dd,1H),6.74(d,1H),6.13(dd,1H),6.20(d,1H) ,1.16(m,6H)

manufacture example 2-11

[0064] Production Example 2-1. Synthesis of 1-chlorohexane

[0065] 1-Hexanol (1.2kg, 11.70mol) and dimethylformamide (DMF, 8.5g, 0.12mol) were stirred and SOCl was added dropwise while maintaining the internal temperature below 30°C 2 (2.1 kg, 17.6 mol). After completion of the dropwise addition, the internal temperature was raised to 80 to 90° C. and stirred for 5 hours. After confirming the completion of the reaction, cooling was performed, and 5 L of purified water was added to separate layers to obtain the title compound (1.3 kg, 94.2%).

[0066] 1 H NMR (CDCl 3 ): 3.49(t,2H), 1.72(m,2H), 1.28(m,2H), 1.27(m,4H), 0.88(m,3H).

manufacture example 2-21

[0067] Production Example 2-2. Synthesis of 1-bromohexane

[0068] 1-Hexanol (1.2 kg, 11.70 mol) and tetrahydrofuran (THF, 6.0 L) were stirred, and PBr was added dropwise while maintaining the internal temperature below 10 °C 3 (3.2 kg, 17.6 mol). After completion of the dropwise addition, the internal temperature was maintained at 10° C. or lower and stirred for 3 hours. After confirming the completion of the reaction, 5 L of purified water was thrown in and the layer was separated to obtain the title compound (1.8 kg, 91.4%).

[0069] 1 H NMR (CDCI 3 ): 3.40(t,2H), 1.85(m,2H), 1.43(m,2H), 1.31(m,4H), 0.90(m,3H).

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

PropertyMeasurementUnit
Bulk densityaaaaaaaaaa
Bulk densityaaaaaaaaaa
Bulk densityaaaaaaaaaa
Login to view more

Abstract

The present invention relates to a method for preparing diethylamino hydroxybenzoyl hexyl benzoate and, specifically, to: a method for preparing diethylamino hydroxybenzoyl hexyl benzoate, which has a simple preparation process and can be commercially mass produced; and crystalline diethylamino hydroxybenzoyl hexyl benzoate particles prepared thereby. According to the present invention, crystalline diethylamino hydroxybenzoyl hexyl benzoate particles having an excellent ultraviolet blocking effect can be stably obtained in a high yield.

Description

technical field [0001] The present invention relates to a kind of manufacturing method of diethylamino hydroxybenzoyl hexyl benzoate, in particular to a kind of manufacturing method of diethylamino hydroxy benzoyl hexyl benzoate which is easy to manufacture and can realize commercial mass production , A method for producing crystalline particles of diethylaminohydroxybenzoylhexylbenzoate, and diethylaminohydroxybenzoylhexylbenzoate produced by the production method. Background technique [0002] All ultraviolet rays, including those contained in sunlight, are carcinogens. The International Agency for Research on Cancer, or IARC, classifies all types of UV rays as Group I carcinogens, ie substances known to induce cancer. [0003] In addition to being carcinogenic, UV rays can damage the skin, eyes and immune system and induce skin aging. In theory, aging can be delayed by 27 times when it is not exposed to ultraviolet light. In particular, a large amount of UV-B (320nm~28...

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
IPC IPC(8): C07C213/06C07C219/34C07C213/10C07C221/00C07C225/22C07C229/52C07C227/14
CPCC07C227/18C07C229/52C07C213/06C07C219/34C07C213/10
Inventor 尹种培白弦玗崔银花
Owner AS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