1-Bromo-3-chloropropane → Toluene-4-thiosulfonic acid S-(3-chloropropyl)ester

HRID 707674노트

반응식

HRID 707674 반응식
[S:1]([C:5]1[CH:11]=[CH:10][C:8]([CH3:9])=[CH:7][CH:6]=1)([O-:4])(=[O:3])=[S:2].[K+].Br[CH2:14][CH2:15][CH2:16][Cl:17]>CC(C)=O>[Cl:17][CH2:16][CH2:15][CH2:14][S:2][S:1]([C:5]1[CH:11]=[CH:10][C:8]([CH3:9])=[CH:7][CH:6]=1)(=[O:4])=[O:3]

참가 물질

4

반응물 2

HCID 80061-Bromo-3-chloropropaneHCID 23662126Benzenesulfonothioic acid, 4-methyl-, potassium salt (1:1)

생성물 1

HCID 67607671Toluene-4-thiosulfonic acid S-(3-chloropropyl)ester

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Potassium thiotosylate (50.0 g, 221 mmol, 1.0 eq.) and 1-bromo-3-chloropropane (38.0 g, 241 mmol, 1.09 eq.) were stirred together in acetone (1 L) at room temperature for 72 hours. The mixture was then concentrated. Next, the mixture was partitioned between dichloromethane and water. The organic solution was washed with brine (2×), dried using MgSO4, concentrated and azeotroped with toluene to produce a pale yellow oil weighing 54 g (92%).

후처리

  1. concentrationThe mixture was then concentrated
  2. customNext, the mixture was partitioned between dichloromethane and water
  3. washThe organic solution was washed with brine (2×)
  4. customdried
  5. concentrationconcentrated
  6. customazeotroped with toluene
  7. customto produce a pale yellow oil

출처 및 근거

ORD 기록
ord-0426f9cb8c95443eafe75af8829db2b2
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09175042B2

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