Maleic Acid → 7-Chloro-3-(5-dimethylaminomethyl-[1,2,4]oxadiazol-3-yl)-5-methyl-4,5-dihydro-imidazo[1,5-a][1,4]benzodiazepin-6-one maleate

HRID 1936550ノート

反応式

HRID 1936550 の反応式
[Cl:1][C:2]1[C:7]2[C:8](=[O:26])[N:9]([CH3:25])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[N:20]=[C:19]([CH2:21][N:22]([CH3:24])[CH3:23])[O:18][N:17]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1.[C:27]([OH:34])(=[O:33])/[CH:28]=[CH:29]\[C:30]([OH:32])=[O:31]>C(O)C>[C:27]([OH:34])(=[O:33])/[CH:28]=[CH:29]\[C:30]([OH:32])=[O:31].[Cl:1][C:2]1[C:7]2[C:8](=[O:26])[N:9]([CH3:25])[CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]3[N:20]=[C:19]([CH2:21][N:22]([CH3:23])[CH3:24])[O:18][N:17]=3)[C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 444266Maleic AcidHCID 9885841Evt-201

生成物 1

HCID 700019197-Chloro-3-(5-dimethylaminomethyl-[1,2,4]oxadiazol-3-yl)-5-methyl-4,5-dihydro-imidazo[1,5-a][1,4]benzodiazepin-6-one maleate収率 94.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

373 mg 7-Chloro-3-(5-dimethylaminomethyl-[1,2,4]oxadiazol-3-yl)-5-methyl-4,5-dihydro-imidazo[1,5-a][1,4]benzodiazepin-6-one (I) and 116 mg maleic acid were dissloved in 3 ml hot ethanol. The salt crystalized on cooling. The suspension was stirred for 10 min at 0° C. Filtration and drying afforded 460 mg 7-Chloro-3-(5-dimethylaminomethyl-[1,2,4]oxadiazol-3-yl)-5-methyl-4,5-dihydro-imidazo[1,5-a][1,4]benzodiazepin-6-one maleate (1:1) as a whit solid. m.p. 182-184° C.

後処理

  1. customThe salt crystalized
  2. temperatureon cooling
  3. filtrationFiltration
  4. customdrying

出典と根拠

ORDレコード
ord-c9165490fd954268ad07e715f0d044d3
出典データセット
uspto-grants-2002_05
特許番号
US06391873B1

反応ノート

読み込み中…