Chloroform → 7-Trifluoromethyl-8,10-dichloro-10,11-dihydrodibenzo(b,f)thiepine

HRID 1732769ノート

反応式

HRID 1732769 の反応式
[F:1][C:2]([F:20])([F:19])[C:3]1[CH:4]=[C:5]([S:10][C:11]2[CH:18]=[CH:17][CH:16]=[CH:15][C:12]=2[CH2:13]O)[CH:6]=[CH:7][C:8]=1[Cl:9].S(Cl)(Cl)=O.[CH:25](Cl)(Cl)[Cl:26]>>[F:1][C:2]([F:20])([F:19])[C:3]1[C:8]([Cl:9])=[CH:7][C:6]2[CH:25]([Cl:26])[CH2:13][C:12]3[CH:15]=[CH:16][CH:17]=[CH:18][C:11]=3[S:10][C:5]=2[CH:4]=1

参加物

4

反応物 3

HCID 6212ChloroformHCID 24386Thionyl ChlorideHCID 12374606(2-{[4-Chloro-3-(trifluoromethyl)phenyl]sulfanyl}phenyl)methanol

生成物 1

HCID 123746247-Trifluoromethyl-8,10-dichloro-10,11-dihydrodibenzo(b,f)thiepine

実験手順

A mixture of the alcohol from the preceding experiment (3.3 g) and thionyl chloride (1.2 ml) is allowed to stand at room temperature for 12 hours and then heated under a reflux condenser in a steam-bath for 1 hour. The reaction mixture is cooled, dissolved in chloroform and the solution washed with water and dried over calcium chloride. Evaporation of the solvent affords crystalline 7-trifluoromethyl-8,10-dichloro-10,11-dihydrodibenzo(b,f)thiepine, melting at 100°-102° C. after crystallization from acetone.

後処理

  1. temperatureheated under a reflux condenser in a steam-bath for 1 hour
  2. temperatureThe reaction mixture is cooled
  3. washthe solution washed with water
  4. dry with materialdried over calcium chloride
  5. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-d62f93ef8f1649088421046c2c9926d3
出典データセット
uspto-grants-1980_12
特許番号
US04238611

反応ノート

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