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1-Methyl-2-imidazolecarboxaldehyde → HCID 89420968, 화합물

HRID 246201
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HRID 246201 반응식
[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[C:3]1[CH:7]=O.[CH3:9][C:10]([S:13]([NH2:15])=[O:14])([CH3:12])[CH3:11]>ClCCl>[CH3:1][N:2]1[CH:6]=[CH:5][N:4]=[C:3]1/[CH:7]=[N:15]/[S:13]([C:10]([CH3:12])([CH3:11])[CH3:9])=[O:14]
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참가 물질

4

반응물 2

HCID 1395751-Methyl-2-imidazolecarboxaldehydeHCID 3382465Tert-Butanesulfinamide

생성물 1

HCID 89420968HCID 89420968, 화합물수율 76.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
25 °C

실험 절차

In a 25 mL vial, cupric sulfate (1.96 g, 12.3 mmol), 1-methyl-1H-imidazole-2-carbaldehyde (450 mg, 4.09 mmol) and 2-methylpropane-2-sulfinamide (594 mg, 4.9 mmol) were combined with dichloromethane (2 ml) to give a light blue suspension. The reaction mixture was stirred at 25° C. for 15 h then filtered through Celite. The reaction mixture was filtered again through silica gel eluting with ethyl acetate. The crude reaction mixture was concentrated in vacuo to provide 670 mg (76%) of 2-methyl-propane-2-sulfinic acid 1-(1-methyl-1H-imidazol-2-yl)-meth-(E)-ylideneamide as an oil. 1H NMR (300 MHz, CDCl3): δ 8.62 (s, 1H), 7.27 (bs, 1H), 7.08 (bs, 1H), 4.02 (s, 1H), 1.26 (s, 9H).

후처리

  1. customto give a light blue suspension
  2. filtrationthen filtered through Celite
  3. filtrationThe reaction mixture was filtered again through silica gel eluting with ethyl acetate
  4. customThe crude reaction mixture
  5. concentrationwas concentrated in vacuo

출처 및 근거

ORD 기록
ord-ce804fb0d3a144c1acba6c8f7b12f4fe
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658646B2

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