Water → 2-Hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin

HRID 866936

반응식

HRID 866936 반응식
[OH-:1].[Na+].C[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)COCCO>[OH: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 14798Sodium HydroxideHCID 233370482-Methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin

생성물 1

HCID 233370412-Hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin수율 46%

시약·촉매·용매 1

HCID 8117Diethylene Glycol용매

반응 조건

온도
200 °C

실험 절차

An amount of 2.2g of sodium hydroxide was dissolved in 30ml of diethylene glycol by application of heat and to the mixture was added 2.2g of 2-methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin and the resulting mixture was stirred at 200° C for 16 hours. After cooling, to the mixture was added water and the mixture was extracted with ethyl acetate. The equeous layer was acidified with conc. hydrochloric acid and extracted with ethyl acetate. This extract was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and freed of the solvent to obtain the residue. This residue was recrystallized from benzene to afford 1.1g (46%) of 2-hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin as brown crystals having a melting point of 210°-211° C.

후처리

  1. temperatureof heat and to the mixture
  2. temperatureAfter cooling, to the mixture
  3. extractionthe mixture was extracted with ethyl acetate
  4. extractionextracted with ethyl acetate
  5. washThis extract was washed with saturated sodium chloride solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. customto obtain the residue
  8. customThis residue was recrystallized from benzene

출처 및 근거

ORD 기록
ord-9ddbed6ebfaa4e00a04faccfdbc7a43c
출처 데이터셋
uspto-grants-1978_07
특허 번호
US04101667

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