Potassium thiocyanate → (+/-)-8-Methyl-5-(4-nitrophenyl)-7-thiocarbamoyl-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine

HRID 25057

反応式

HRID 25057 の反応式
[S-:1][C:2]#[N:3].[K+].[CH3:5][CH:6]1[CH2:12][C:11]2[CH:13]=[C:14]3[O:19][CH2:18][O:17][C:15]3=[CH:16][C:10]=2[C:9]([C:20]2[CH:25]=[CH:24][C:23]([N+:26]([O-:28])=[O:27])=[CH:22][CH:21]=2)=[N:8][NH:7]1>C(O)(=O)C>[CH3:5][CH:6]1[CH2:12][C:11]2[CH:13]=[C:14]3[O:19][CH2:18][O:17][C:15]3=[CH:16][C:10]=2[C:9]([C:20]2[CH:25]=[CH:24][C:23]([N+:26]([O-:28])=[O:27])=[CH:22][CH:21]=2)=[N:8][N:7]1[C:2](=[S:1])[NH2:3]

参加物

4

反応物 2

HCID 516872Potassium thiocyanateHCID 103364221-(4-Nitrophenyl)-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine

生成物 1

HCID 12137394(+/-)-8-Methyl-5-(4-nitrophenyl)-7-thiocarbamoyl-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine収率 76.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
105 °C

実験手順

A mixture of 0.90 g (9.26 mmol) of potassium thiocyanate, 2.00 g (6.15 mmol) of (±)-8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine and 40 ml of acetic acid was stirred at 100-110° C. for 6 h. After cooling, the precipitated crystals were filtered off, washed with water and dried to yield 1.80 g (76%) of the title compound. Mp.: 242-243° C.

後処理

  1. temperatureAfter cooling
  2. filtrationthe precipitated crystals were filtered off
  3. washwashed with water
  4. customdried

出典と根拠

ORDレコード
ord-58a86a71215a45fa83174b0b3f868e5d
出典データセット
uspto-grants-2005_02
特許番号
US06858605B2

関連ノート

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