37441-16-0 → HCID 44128653、化合物

HRID 2098303ノート

反応式

HRID 2098303 の反応式
[N:1]([CH2:4][CH2:5][S:6][CH3:7])=[C:2]=[O:3].[N+:8](=[C:10]1[N:14]=[CH:13][N:12]=[C:11]1[C:15]([NH2:17])=[O:16])=[N-:9]>CS(C)=O>[CH3:7][S:6][CH2:5][CH2:4][N:1]1[C:2](=[O:3])[N:14]2[CH:13]=[N:12][C:11]([C:15]([NH2:17])=[O:16])=[C:10]2[N:8]=[N:9]1

参加物

4

反応物 2

HCID 1787232937441-16-0HCID 534265854-Diazo-4H-imidazole-5-carboxamide

生成物 1

HCID 44128653HCID 44128653、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

1-Isocyanato-2-methylsulfanyl-ethane (1.09 g, 9.31 mmol) was added drop wise to a suspension of 5-diazoimidazole-4-carboxamide (0.5 g, 3.65 mmol) in dry dimethylsulfoxide (5 mL) at room temperature under nitrogen. The resulting mixture was stirred at room temperature overnight. The reaction was quenched by the addition of ice and the solid product (brown) was removed by filtration, washed with Et2O, and purified using flash chromatography (SiO2) using MeCN:CH2Cl2 (0-100% MeCN) Yield: 52 mg, 26%. 1H NMR (400 MHz, d6-DMSO) δ ppm: 8.87 (1H, s), 7.80 (1H, s), 7.66 (1H, s), 4.48 (2H, t), 2.94 (2H, t).

後処理

  1. customThe reaction was quenched by the addition of ice
  2. customthe solid product (brown) was removed by filtration
  3. washwashed with Et2O
  4. custompurified

出典と根拠

ORDレコード
ord-8be1f7dbadd54db2b4922f226690c6d1
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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