Phosphorus sulfide (P2S5) → 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepine-2-thione

HRID 1580643ノート

反応式

HRID 1580643 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=O)[CH:9]([CH3:13])[N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:22]>N1C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[S:22])[CH:9]([CH3:13])[N:8]=[C:7]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]=2[CH:20]=1

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 382377-chloro-3-methyl-5-phenyl-2,3-dihydro-1H-1,4-benzodiazepin-2-one

生成物 1

HCID 126124347-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepine-2-thione

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A stirred mixture of 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepin-2-one (0.294 mole), dry pyridine (2300 ml.) and phosphorus pentasulfide (72.4 g.; 0.323 mole) is reflexed under nitrogen for 30 minutes, cooled and concentrated in vacuo. A suspension of the residue in ice water is extracted with methylene chloride. The extract is dried over anhydrous potassium carbonate and concentrated. The residue thus obtained is crystallized from methylene chlorideethanol to give 7-chloro-1,3-dihydro-3-methyl-5-phenyl-2H-1,4-benzodiazepine-2-thione.

後処理

  1. temperaturecooled
  2. concentrationconcentrated in vacuo
  3. additionA suspension of the residue in ice water
  4. extractionis extracted with methylene chloride
  5. dry with materialThe extract is dried over anhydrous potassium carbonate
  6. concentrationconcentrated
  7. customThe residue thus obtained
  8. customis crystallized from methylene chlorideethanol

出典と根拠

ORDレコード
ord-98251a72024043dba100ede69d665bbb
出典データセット
uspto-grants-1976_01
特許番号
US03933794

反応ノート

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