4-Diazo-4H-imidazole-5-carboxamide → HCID 44128467、化合物

HRID 2098300ノート

反応式

HRID 2098300 の反応式
[N:1]([CH2:4][C:5]1[O:9][N:8]=[C:7]([CH3:10])[CH:6]=1)=[C:2]=[O:3].[N+:11](=[C:13]1[N:17]=[CH:16][N:15]=[C:14]1[C:18]([NH2:20])=[O:19])=[N-:12]>CS(C)=O>[CH3:10][C:7]1[CH:6]=[C:5]([CH2:4][N:1]2[C:2](=[O:3])[N:17]3[CH:16]=[N:15][C:14]([C:18]([NH2:20])=[O:19])=[C:13]3[N:11]=[N:12]2)[O:9][N:8]=1

参加物

4

反応物 2

HCID 534265854-Diazo-4H-imidazole-5-carboxamideHCID 595674565-(Isocyanatomethyl)-3-methyl-1,2-oxazole

生成物 1

HCID 44128467HCID 44128467、化合物収率 99.9%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒2 回

実験手順

5-Isocyanatomethyl-3-methyl-isoxazole (735 mg, 5.32 mmol) was diluted in DMSO (1.5 mL) and added to a solution of 5-diazoimidazole-4-carboxamide (250 mg, 1.83 mmol) in 2 mL DMSO. The reaction mixture was stirred at room temperature for 16 hours before the addition of sufficient ice water to cause precipitation of the crude product which was collected by vacuum filtration and washed with Et2O (1 reaction volume title compound as a yellow solid (503 mg, 98% yield). 1H NMR (400 MHz, d6-DMSO) δ ppm: 8.86 (1H, s), 7.84 (1H, s), 7.71 (1H, s), 6.51 (1H, s), 5.64 (2H, s), 2.21 (3H, s).

後処理

  1. customprecipitation of the crude product which
  2. filtrationwas collected by vacuum filtration
  3. washwashed with Et2O (

出典と根拠

ORDレコード
ord-eecc681afa584283b7643de9f0f82251
出典データセット
uspto-grants-2013_05
特許番号
US08450479B2

反応ノート

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