2-Trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-on → 2-Trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol

HRID 261560

반응식

HRID 261560 반응식
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:19]=[CH:18][C:6]2[S:7][C:8]3[CH:16]=[CH:15][CH:14]=[C:13]([Cl:17])[C:9]=3[CH2:10][C:11](=[O:12])[C:5]=2[CH:4]=1.B.[Na]>CO>[F:21][C:2]([F:1])([F:20])[C:3]1[CH:19]=[CH:18][C:6]2[S:7][C:8]3[CH:16]=[CH:15][CH:14]=[C:13]([Cl:17])[C:9]=3[CH2:10][CH:11]([OH:12])[C:5]=2[CH:4]=1

참가 물질

4

반응물 2

HCID 126871142-Trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-onHCID 178418435HCID 178418435, 화합물

생성물 1

HCID 126871162-Trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To the mixture of 2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-one obtained in Example 40 and 10 ml of methanol was gradually added 0.2 g of sodium boron hydride with ice-cooling over a period of 5 minutes and the mixture was reacted at room temperature for 30 minutes and refluxed for 15 minutes. After the completion of the reaction, methanol was distilled off. After cooling, to the mixture was added water and the mixture was extracted with chloroform. The extract was washed with water, dried over anhydrous sodium sulfate and freed of the solvent to obtain 0.5 g of 2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol as colorless crystals having a melting point of 130°-132° C.

후처리

  1. temperaturecooling over a period of 5 minutes
  2. customthe mixture was reacted at room temperature for 30 minutes
  3. temperaturerefluxed for 15 minutes
  4. distillationwas distilled off
  5. temperatureAfter cooling, to the mixture
  6. additionwas added water
  7. extractionthe mixture was extracted with chloroform
  8. washThe extract was washed with water
  9. dry with materialdried over anhydrous sodium sulfate

출처 및 근거

ORD 기록
ord-3325dc4f6ce54b34858198213e576066
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04166127

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