Clonazepam → 5-(2-chlorophenyl)-2-[bis(morpholino)phosphinyloxy]-7-nitro-3H-1,4-benzodiazepine

HRID 649265

반응식

HRID 649265 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[NH:12][C:11](=[O:22])[CH2:10][N:9]=1.[H-].[Na+].[H-].[H][H].[O:28]1[CH2:33][CH2:32][N:31]([P:34](Cl)([N:36]2[CH2:41][CH2:40][O:39][CH2:38][CH2:37]2)=[O:35])[CH2:30][CH2:29]1>O1CCCC1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:14]2[CH:15]=[C:16]([N+:19]([O-:21])=[O:20])[CH:17]=[CH:18][C:13]=2[N:12]=[C:11]([O:22][P:34]([N:36]2[CH2:37][CH2:38][O:39][CH2:40][CH2:41]2)([N:31]2[CH2:32][CH2:33][O:28][CH2:29][CH2:30]2)=[O:35])[CH2:10][N:9]=1

참가 물질

7

반응물 5

HCID 2802ClonazepamHCID 24758Sodium hydrideHCID 166653HydrideHCID 12506606Bis(morpholino)phosphinyl chlorideHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 201429915-(2-chlorophenyl)-2-[bis(morpholino)phosphinyloxy]-7-nitro-3H-1,4-benzodiazepine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 4.74 g (15 mmoles) of 5-(2-chlorophenyl)-1,3-dihydro-7-nitro-2H-1,4-benzodiazepin-2-one in 80 ml of dry tetrahydrofuran at room temperature was added 875 mg of a 50% dispersion of sodium hydride in oil (18 mmoles of hydride). The mixtute was stirred at room temperature for 1 hr until hydrogen evolution stopped. Dimorpholinophosphinic chloride (7.5 g, 30 mmoles) was added and the resulting mixture was stirred at room temperature for 3 hrs. Solids (mixture of product and salt) were collected and partitioned between water and methylene chloride. The methylene chloride layer was dried and evaporated. Crystallization of the residue from methylene chloride ether gave colorless needles, mp 214°-216°.

후처리

  1. additionSolids (mixture of product and salt)
  2. customwere collected
  3. custompartitioned between water and methylene chloride
  4. dry with materialThe methylene chloride layer was dried
  5. customevaporated
  6. customCrystallization of the residue from methylene chloride ether
  7. customgave colorless needles, mp 214°-216°

출처 및 근거

ORD 기록
ord-455a76d780e64a069b13066b8c593c22
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04739049

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