Hydrogen Sulfide → (3-Mercaptopropyl)trimethoxysilane

HRID 357671

반응식

HRID 357671 반응식
[SH2:1].Cl[CH2:3][CH2:4][CH2:5][Si:6]([O:11][CH3:12])([O:9][CH3:10])[O:7][CH3:8]>CO>[SH:1][CH2:3][CH2:4][CH2:5][Si:6]([O:11][CH3:12])([O:9][CH3:10])[O:7][CH3:8]

참가 물질

4

반응물 2

HCID 402Hydrogen Sulfide3회HCID 624493-(Trimethoxysilyl)propyl chloride

생성물 1

HCID 20473(3-Mercaptopropyl)trimethoxysilane수율 94.1%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
70 °C

실험 절차

267.6 g of a methanol solution of 22% sodium hydrogensulfide anhydride (1.05 mol) was put into an autoclave with an internal volume of 1 liter, and the air was replaced by nitrogen. 0.3 mol of hydrogen sulfide was then blown in and the system was pressurized to 0.9 kgf/cm2 to oversaturate hydrogen sulfide. After heating the system up to 70° C., 198.7 g (1.0 mole) of 3-chloropropyltrimethoxy silane was dripped for 3 hours, and, during the dripping, 0.05 mol of hydrogen sulfide was blown into the system so that the pressure in the system was kept at 2.5 kgf/cm2. After the dripping, the temperature was raised to 100° C. and the system was aged for 1 hour, followed by cooling. By-product salts produced in the reaction were filtered away. The composition was analyzed by means of gas chromatography. 3-mercaptopropyltrimethoxy silane was obtained with a yield of 94.1%.

후처리

  1. temperatureAfter the dripping, the temperature was raised to 100° C.
  2. temperatureby cooling
  3. customBy-product salts produced in the reaction
  4. filtrationwere filtered away

출처 및 근거

ORD 기록
ord-5b5525a8619d4f268478995675378308
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840952

연결된 노트

불러오는 중…