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

HRID 435721노트

반응식

HRID 435721 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
30 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3898586fd24444b090adf8d1f07128fc
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04006144

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