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

HRID 1580643노트

반응식

HRID 1580643 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-98251a72024043dba100ede69d665bbb
출처 데이터셋
uspto-grants-1976_01
특허 번호
US03933794

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