4-Diazo-4H-imidazole-5-carboxamide → HCID 44128467, 화합물

HRID 2098300노트

반응식

HRID 2098300 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 44128467HCID 44128467, 화합물수율 99.9%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-eecc681afa584283b7643de9f0f82251
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08450479B2

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