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Dimethylformamide → HCID 67037586, 화합물

HRID 1723659
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HRID 1723659 반응식
[CH:1]1([N:5]2[CH:9]=[C:8](C(=O)C)[N:7]=[C:6]2[CH3:13])[CH2:4][CH2:3][CH2:2]1.[CH3:14][C:15]([N:17]([CH3:19])[CH3:18])=O.CN([CH:23]=[O:24])C>>[CH3:18][N:17]([CH3:19])[CH:15]=[CH:14][C:23]([C:9]1[N:5]([CH:1]2[CH2:2][CH2:3][CH2:4]2)[C:6]([CH3:13])=[N:7][CH:8]=1)=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 6228DimethylformamideHCID 31374DimethylacetamideHCID 688810941-Cyclobutyl-2-methyl-4-acetylimidazole

생성물 1

HCID 67037586HCID 67037586, 화합물수율 47%

실험 절차

1-Cyclobutyl-2-methyl-4-acetylimidazole (Method 3; 2.52 g, 14.1 mmol) was dissolved in DMF.DMA (75 mL) and the mixture heated at reflux, under an atmosphere of nitrogen, for 54 hours. The reaction mixture was allowed to cool to ambient temperature the product crystallised. The solid product was collected by filtration, washed with DMF.DMA and then ether and dried under vacuum at 40° C. to give the title compound (1.55 g, 47%) as a pale brown crystalline solid. NMR: 1.72 (m, 2H), 2.28 (m, 2H), 2.39 (s, 3H), 2.64 (m, 2H), 2.95 (m, 6H), 5.22 (m, 1H), 5.50 (d, 1H), 7.39 (s, 1H), 7.51 (d, 1H).

후처리

  1. temperatureat reflux, under an atmosphere of nitrogen, for 54 hours
  2. customcrystallised
  3. filtrationThe solid product was collected by filtration
  4. washwashed with DMF
  5. dry with materialDMA and then ether and dried under vacuum at 40° C.

출처 및 근거

ORD 기록
ord-0ffa5dac74b64c51b39a39b1efa6292b
출처 데이터셋
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07485638B2

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