Water → 10,11-Dihydro-2-trifluoromethyl-dibenzo[b,f]thiepin-10-ol

HRID 435721ノート

反応式

HRID 435721 の反応式
[F:1][C:2]([F:20])([F:19])[C:3]1[CH:18]=[CH:17][C:6]2[S:7][C:8]3[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=3[C:10](=[O:12])[CH2:11][C:5]=2[CH:4]=1.[BH4-].[Na+].O.C(Cl)(Cl)Cl>C(O)C>[F:20][C:2]([F:1])([F:19])[C:3]1[CH:18]=[CH:17][C:6]2[S:7][C:8]3[CH:16]=[CH:15][CH:14]=[CH:13][C:9]=3[CH:10]([OH:12])[CH2:11][C:5]=2[CH:4]=1

参加物

6

反応物 4

HCID 962WaterHCID 6212ChloroformHCID 4311764Sodium borohydrideHCID 1222396810,11-Dihydro-2-trifluoromethyl-dibenzo[b,f]-thiepin-10-one

生成物 1

HCID 1222397310,11-Dihydro-2-trifluoromethyl-dibenzo[b,f]thiepin-10-ol

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
30 °C

実験手順

12 g of 10,11-dihydro-2-trifluoromethyl-dibenzo[b,f]thiepin-10-one are dissolved in 110 ml of absolute ethanol and treated with 4 g of sodium borohydride. The mixture is held at reflux for 12 minutes, cooled to 30° C and treated with 350 ml of water and 100 ml of chloroform. After equilibration, the organic phase is washed with aqueous sodium chloride solution, dried over sodium sulphate and evaporated under reduced pressure. There is obtained 10,11-dihydro-2-trifluoromethyl-dibenzo[b,f]thiepin-10-ol in the form of yellow crystals which melt at 122°-123° C.

後処理

  1. temperatureat reflux for 12 minutes
  2. washAfter equilibration, the organic phase is washed with aqueous sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-3898586fd24444b090adf8d1f07128fc
出典データセット
uspto-grants-1977_02
特許番号
US04006144

反応ノート

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