반응 #471752

반응 방정식

3-(amino)propyltrimethoxysilane

triethylamine

methacryloyl chloride

→

product

수율 71.6%

3-(methacrylamido)propyltrimethoxysilane

수율 71.6%

용매

dichloromethane

반응 조건

후처리

1. 1
   여과The precipitated hydrochloride was filtered off
2. 2
   세척washed with dichloromethane
3. 3
   기타The volatile constituents were removed at 40° C. under reduced pressure
4. 4
   기타the rotary evaporator
5. 5
   기타A yellow liquid with precipitated solid (hydrochloride)
6. 6
   기타The precipitation of the hydrochloride
7. 7
   workup.ADDITIONby adding 150 ml diethyl ether
8. 8
   여과the precipitate was filtered off
9. 9
   농축the filtrate concentrated at 40° C.
10. 10
    기타a rotary evaporator with introduction of dry air
11. 11
    workup.DISTILLATIONthe raw product (104.2 g) was distilled at a pressure of 6×10−4 mbar

실험 절차

77.4 g 3-(amino)propyltrimethoxysilane, 43.7 g triethylamine and 25 mg di-tert.-butyl-p-cresol were dissolved under argon in 500 ml dichloromethane. 45.1 g methacryloyl chloride was slowly added dropwise at −5° C. within 1 h, and the whole was then stirred for 1 h at 0° C. The precipitated hydrochloride was filtered off and washed with dichloromethane. The volatile constituents were removed at 40° C. under reduced pressure using the rotary evaporator. A yellow liquid with precipitated solid (hydrochloride) remained. The precipitation of the hydrochloride was completed by adding 150 ml diethyl ether, the precipitate was filtered off and the filtrate concentrated at 40° C. using a rotary evaporator with introduction of dry air. The brownish liquid was freed of residual volatile constituents at 4×10−2 mbar, and the raw product (104.2 g) was distilled at a pressure of 6×10−4 mbar. The product had a boiling point of 123-125° C. 76.4 g of product was obtained as yellowish, clear liquid.

출처