8-chloro-1-methyl-6-phenyl-3,3a,4,6-tetrahydro-5H-imidazo[1,5-a][1,5]benzodiazepin-5-one → 8-Chloro-4,6-dihydro-1-methyl-6-phenyl-5H-imidazo[1,5-a][1,5]benzodiazepin-5-one

HRID 1763251ノート

反応式

HRID 1763251 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:12]([CH3:15])=[N:13][CH2:14][CH:10]3[CH2:9][C:8](=[O:16])[N:7]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[C:6]=2[CH:23]=1>[O-2].[O-2].[Mn+4].C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:12]([CH3:15])=[N:13][CH:14]=[C:10]3[CH2:9][C:8](=[O:16])[N:7]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:6]=2[CH:23]=1

参加物

4

反応物 1

HCID 227495508-chloro-1-methyl-6-phenyl-3,3a,4,6-tetrahydro-5H-imidazo[1,5-a][1,5]benzodiazepin-5-one

生成物 1

HCID 227495468-Chloro-4,6-dihydro-1-methyl-6-phenyl-5H-imidazo[1,5-a][1,5]benzodiazepin-5-one

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒HCID 1140Toluene溶媒

実験手順

A mixture of 7.2 g (0.022 moles) of 8-chloro-1-methyl-6-phenyl-3,3a,4,6-tetrahydro-5H-imidazo[1,5-a][1,5]benzodiazepin-5-one, 45 g of activated manganese dioxide and 1.5 l. of toluene was stirred and refluxed for 45 minutes. The manganese dioxide was filtered off and washed well with tetrahydrofuran and methylene chloride. The filtrate was evaporated and the residue was crystallized from ethyl acetate to yield end product with mp 276°-278° C.

後処理

  1. temperaturerefluxed for 45 minutes
  2. filtrationThe manganese dioxide was filtered off
  3. washwashed well with tetrahydrofuran and methylene chloride
  4. customThe filtrate was evaporated
  5. customthe residue was crystallized from ethyl acetate
  6. customto yield end product with mp 276°-278° C.

出典と根拠

ORDレコード
ord-b2280064700b4bd081c0dd38020f1f99
出典データセット
uspto-grants-1978_09
特許番号
US04111931

反応ノート

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