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

HRID 2259405ノート

反応式

HRID 2259405 の反応式
[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

参加物

5

反応物 3

HCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 53400706HCID 53400706、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fc6c6655846d4acfaf8a67555ceb05d1
出典データセット
uspto-grants-1995_12
特許番号
US05473066

反応ノート

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