Water → Dibenzo(b,f)thiepin-1-carboxylic acid, 10,11-dihydro-8-methoxy-

HRID 903654

반응식

HRID 903654 반응식
[OH-:1].[K+].[CH3:3][O:4][C:5]1[CH:21]=[CH:20][C:8]2[S:9][C:10]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]#N)[C:11]=3[CH2:12][CH2:13][C:7]=2[CH:6]=1.[OH2:22]>C(O)C>[CH3:3][O:4][C:5]1[CH:21]=[CH:20][C:8]2[S:9][C:10]3[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([OH:22])=[O:1])[C:11]=3[CH2:12][CH2:13][C:7]=2[CH:6]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 233370482-Methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin

생성물 1

HCID 3045903Dibenzo(b,f)thiepin-1-carboxylic acid, 10,11-dihydro-8-methoxy-수율 69%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

An amount of 6.0 g potassium hydroxide was dissolved in 20 ml of 80% ethanol and to the solution was added 1 g of 2-methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin and the resulting mixture was refluxed for 26 hours. The mixture was freed of the solvent under reduced pressure to obtain the residue, which was dissolved in water and extracted with ethyl acetate. The aqueous layer was acidified with conc. hydrochloric acid and extracted with ethyl acetate. The extract was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and freed of the solvent to give 743 mg (69%) of 2-methoxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin as pale reddish needles having a melting point of 185°-186° l C.

후처리

  1. temperaturethe resulting mixture was refluxed for 26 hours
  2. customto obtain the residue, which
  3. extractionextracted with ethyl acetate
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with saturated sodium chloride solution
  6. dry with materialdried over anhydrous sodium sulfate

출처 및 근거

ORD 기록
ord-d4a7710c4f1d49358b6f65b26946471e
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04228284

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