Pyridine → 2H-1,5-Benzodiazepine-2-thione, 1,3-dihydro-4-phenyl-

HRID 1112582ノート

反応式

HRID 1112582 の反応式
[C:1]1([C:7]2[CH2:13][C:12](=O)[NH:11][C:10]3[CH:15]=[CH:16][CH:17]=[CH:18][C:9]=3[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:20].N1C=CC=CC=1>O>[C:1]1([C:7]2[CH2:13][C:12](=[S:20])[NH:11][C:10]3[CH:15]=[CH:16][CH:17]=[CH:18][C:9]=3[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 14817Phosphorus sulfide (P2S5)HCID 1777464-Phenyl-3H-1,5-benzodiazepin-2-ol

生成物 1

HCID 30329842H-1,5-Benzodiazepine-2-thione, 1,3-dihydro-4-phenyl-

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 23.6 parts of 2,3-dihydro-4-phenyl-1H-1,5-benzodiazepin-2-one and 24.4 parts of phosphorus pentasulfide in 400 parts by volume of pyridine is stirred at reflux temperature for one hour. This solution is then added dropwise with stirring to about 2000 parts by volume of 60° C. warm water. The solid which forms is separated by filtration, washed with water and dried in air overnight. The product thus obtained is recrystallized from ethyl acetate to give, as beige crystals, 2,3-dihydro-4-phenyl-1H-1,5-benzodiazepine-2-thione. This product has the formula ##STR12##

後処理

  1. temperatureat reflux temperature for one hour
  2. additionThis solution is then added dropwise
  3. stirringwith stirring to about 2000 parts by volume of 60° C.
  4. customThe solid which forms is separated by filtration
  5. washwashed with water
  6. customdried in air overnight
  7. customThe product thus obtained
  8. customis recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-8cae5124a0ea4ef08e21999caaad123b
出典データセット
uspto-grants-1978_10
特許番号
US04123430

反応ノート

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