Water → 4,8-Bis(trifluoromethyl)-10,11-dihydrodibenzo[b,f][1,4]thiazepin-11-thione

HRID 1082076

반응식

HRID 1082076 반응식
[F:1][C:2]([F:24])([F:23])[C:3]1[C:13]2[S:12][C:11]3[CH:14]=[CH:15][C:16]([C:18]([F:21])([F:20])[F:19])=[CH:17][C:10]=3[NH:9][C:8](=O)[C:7]=2[CH:6]=[CH:5][CH:4]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:26].O>N1C=CC=CC=1>[F:1][C:2]([F:24])([F:23])[C:3]1[C:13]2[S:12][C:11]3[CH:14]=[CH:15][C:16]([C:18]([F:21])([F:20])[F:19])=[CH:17][C:10]=3[NH:9][C:8](=[S:26])[C:7]=2[CH:6]=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 14817Phosphorus sulfide (P2S5)HCID 199694574,8-Bis(trifluoromethyl)-10,11-dihydrodibenzo[b,f][1,4]thiazepin-11-one

생성물 1

HCID 233620044,8-Bis(trifluoromethyl)-10,11-dihydrodibenzo[b,f][1,4]thiazepin-11-thione수율 50.8%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

4,8-Bis(trifluoromethyl)-10,11-dihydrodibenzo[b,f][1,4]thiazepin-11-one (0.54 g) was dissolved in pyridine (15 ml). Phosphorus pentasulphide (0.60 g) was added to the solution and the whole was stirred under reflux for 6 hours, then cooled and left overnight. Addition of water (40 ml) and cooling gave a yellow solid which was filtered off, washed with water and recrystallised from ethanol to give the product as yellow needles (0.26 g, m/s. M- =379).

후처리

  1. temperatureunder reflux for 6 hours
  2. temperaturecooled
  3. temperaturecooling
  4. customgave a yellow solid which
  5. filtrationwas filtered off
  6. washwashed with water
  7. customrecrystallised from ethanol

출처 및 근거

ORD 기록
ord-1fe3702d00fa43e08fd4e1296acf6dd0
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05589474

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