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

HRID 1082076

反応式

HRID 1082076 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1fe3702d00fa43e08fd4e1296acf6dd0
出典データセット
uspto-grants-1996_12
特許番号
US05589474

関連ノート

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