Thionyl Chloride → 1-(Chloromethyl)-2-(methylsulfanyl)benzene

HRID 2303439노트

반응식

HRID 2303439 반응식
O[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[S:9][CH3:10].O=S(Cl)[Cl:13]>C(Cl)Cl>[Cl:13][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[S:9][CH3:10]

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 3551404(2-Methylsulfanylphenyl)methanol

생성물 1

HCID 124145821-(Chloromethyl)-2-(methylsulfanyl)benzene

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

2-Hydroxymethyl-1-methylthiobenzene (3.3 g, 21 mmol) is dissolved in 20 ml of absolute CH2Cl2 under an argon atmosphere. A solution of SOCl2 (2.6 g, 21 mmol) in 10 ml of absolute CH2Cl2 is added dropwise with stirring to this initial mixture in the course of 15 min, first under reflux, then at an internal temperature of 30° C. The reaction mixture is stirred under reflux for 2.25 h. The reaction mixture is concentrated and the oily crude product is purified by bulb tube distillation (7.9×10−2 mbar, 125-140° C.): colorless oil; yield: 3.3 g (88%).

후처리

  1. temperaturefirst under reflux
  2. customat an internal temperature of 30° C
  3. temperatureunder reflux for 2.25 h
  4. concentrationThe reaction mixture is concentrated
  5. customthe oily crude product is purified by bulb tube
  6. distillationdistillation (7.9×10−2 mbar, 125-140° C.)

출처 및 근거

ORD 기록
ord-ae0945fb2ca344caaf5993620ddfea24
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06432988B1

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