Hydrogen Sulfide → (3-Mercaptopropyl)trimethoxysilane

HRID 357671ノート

反応式

HRID 357671 の反応式
[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]

参加物

4

反応物 2

HCID 402Hydrogen Sulfide3 回HCID 624493-(Trimethoxysilyl)propyl chloride

生成物 1

HCID 20473(3-Mercaptopropyl)trimethoxysilane収率 94.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-5b5525a8619d4f268478995675378308
出典データセット
uspto-grants-1998_11
特許番号
US05840952

反応ノート

読み込み中…