1-Bromo-3-chloropropane → 6-Chloro-3-(3-chloropropyl)-2(3H)-benzothiazolone

HRID 2259405노트

반응식

HRID 2259405 반응식
[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]=[CH:7][S:8](=O)[C:4]=2[CH:3]=1.C([O-])([O-])=[O:13].[K+].[K+].Br[CH2:19][CH2:20][CH2:21][Cl:22]>CC(C)=O>[Cl:1][C:2]1[CH:11]=[CH:10][C:5]2[N:6]([CH2:19][CH2:20][CH2:21][Cl:22])[C:7](=[O:13])[S:8][C:4]=2[CH:3]=1

참가 물질

5

반응물 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 53400706HCID 53400706, 화합물

생성물 1

HCID 190035086-Chloro-3-(3-chloropropyl)-2(3H)-benzothiazolone수율 93.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A solution of 6-chloro-benzothiazolone (VIII) (55.7 g, 0.3 mol), K2CO3 (62.1 g, 0.45 mol) and 1-bromo-3-chloropropane (IX) (71 g, 0.45 mol) in acetone (600 ml) was refluxed for 16 hours. After cooling, the inorganic substance was filtered off and washed dichloromethane. The filtrate and washings were combined and evaporated in vacuo. The residue was washed with hexane and recrystallized from dichloromethane to obtain compound (X) (73.5 g, yield=93.4%) as colorless needle-shaped crystals.

후처리

  1. temperatureAfter cooling
  2. filtrationthe inorganic substance was filtered off
  3. washwashed dichloromethane
  4. customevaporated in vacuo
  5. washThe residue was washed with hexane
  6. customrecrystallized from dichloromethane

출처 및 근거

ORD 기록
ord-fc6c6655846d4acfaf8a67555ceb05d1
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05473066

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