Hydrogen Sulfide → Thionordiazepam

HRID 649261

반응식

HRID 649261 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10](OP(N3CCOCC3)(N3CCOCC3)=O)[CH2:9][N:8]=[C:7]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:6]=2[CH:33]=1.[SH2:34]>O1CCCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[S:34])[CH2:9][N:8]=[C:7]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:6]=2[CH:33]=1

참가 물질

4

반응물 2

HCID 402Hydrogen SulfideHCID 149078867-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepin

생성물 1

HCID 826706Thionordiazepam

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 245 mg. (0.5 mmole) of 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepine in 10 ml. of tetrahydrofuran containing 0.5 ml. of triethylimine at room temperature was introduced a stream of hydrogen sulfide gas until tlc indicated that all the starting material was consumed (15 minutes). Tetrahydrofuran was evaporated. The residue was partitioned between methylene chloride and water. The methylene chloride layer was dried and evaporated. Crystallization of the residue from methanol yielded, in two crops, a product having a melting point of 243°-245°.

후처리

  1. customwas consumed (15 minutes)
  2. customTetrahydrofuran was evaporated
  3. customThe residue was partitioned between methylene chloride and water
  4. dry with materialThe methylene chloride layer was dried
  5. customevaporated
  6. customCrystallization of the residue from methanol
  7. customyielded, in two crops

출처 및 근거

ORD 기록
ord-3003a7854e9646f68410136383523365
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04739049

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