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Methanol → (+/-)-8-Methyl-7-(2-methyl-3-oxo-2,3-dihydro-1,2,4-thiadiazol-5-yl)-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

HRID 25080
ノート
印刷プレビュー

反応式

HRID 25080 の反応式
[CH3:1][NH:2][C:3]([NH:5][C:6]([N:8]1[CH:14]([CH3:15])[CH2:13][C:12]2[CH:16]=[C:17]3[O:22][CH2:21][O:20][C:18]3=[CH:19][C:11]=2[C:10]([C:23]2[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[CH:25][CH:24]=2)=[N:9]1)=[S:7])=[O:4].BrBr.CO>C(Cl)(Cl)Cl>[CH3:15][CH:14]1[CH2:13][C:12]2[CH:16]=[C:17]3[O:22][CH2:21][O:20][C:18]3=[CH:19][C:11]=2[C:10]([C:23]2[CH:28]=[CH:27][C:26]([N+:29]([O-:31])=[O:30])=[CH:25][CH:24]=2)=[N:9][N:8]1[C:6]1[S:7][N:2]([CH3:1])[C:3](=[O:4])[N:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 24408BromineHCID 86593814(+/-)-1-Methyl-3-{8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carbothioyl}-urea

生成物 1

HCID 22565496(+/-)-8-Methyl-7-(2-methyl-3-oxo-2,3-dihydro-1,2,4-thiadiazol-5-yl)-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine収率 82%

試薬・触媒・溶媒 1

HCID 6212
Chloroform
溶媒
3 回

実験手順

To an ice cooled stirred solution of 0.44 g (1.0 mmol) of the starting material XXVII in 8 ml of chloroform a solution of 0.19 g (1.2 mmol) of bromine in 3 ml of chloroform was added. After 0.5 h the reaction mixture was diluted with 15 ml of chloroform and washed with sodium hydrogen carbonate solution and water. The residue obtained on concentration was stirred with methanol and filtered to yield 0.36 g (82%) of the title compound. Mp.: 296° C. after recrystallization from ethyl acetate.

後処理

  1. additionwas added
  2. washwashed with sodium hydrogen carbonate solution and water
  3. customThe residue obtained on concentration
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-20f6119f8dc742118769727308234a2c
出典データセット
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06858605B2

反応ノート

読み込み中…

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