Dimethylformamide → HCID 68358103, 화합물

HRID 1406004노트

반응식

HRID 1406004 반응식
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9][CH3:10])[C:4]=1[NH:11][C:12]([C:14]1[C:15]2[CH2:23][CH2:22][CH2:21][CH2:20][C:19](=[O:24])[C:16]=2[NH:17][N:18]=1)=[O:13])[CH3:2].[CH3:25]N(C=O)C.CI>CCOC(C)=O>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH2:9][CH3:10])[C:4]=1[NH:11][C:12]([C:14]1[C:15]2[CH2:23][CH2:22][CH2:21][CH2:20][C:19](=[O:24])[C:16]=2[N:17]([CH3:25])[N:18]=1)=[O:13])[CH3:2]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 178436232HCID 178436232, 화합물

생성물 1

HCID 68358103HCID 68358103, 화합물수율 91%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of N-(2,6-diethylphenyl)-8-oxo-1,4,5,6,7,8-hexahydrocyclohepta[c]pyrazole-3-carboxamide (1.04 g, 3.211 mmol) in DMF (12 mL) Cs2CO3 (1.255 g, 3.85 mmol) and methyl iodide (0.22 mL, 3.532 mmol) were added. The reaction was stirred at room temperature for 1 h, then AcOEt (60 mL) was added and the organic phase washed with water (3×50 mL). The organic fraction was dried over Na2SO4, filtered, and concentrated in vacuo. Purification by flash chromatography on silica gel (eluant: AcOEt/hexane 1/9) provided 0.99 g (91% yield) of the title compound as a white solid.

후처리

  1. washthe organic phase washed with water (3×50 mL)
  2. dry with materialThe organic fraction was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customPurification by flash chromatography on silica gel (eluant: AcOEt/hexane 1/9)

출처 및 근거

ORD 기록
ord-30c2bef9b6b54858a0e5a74e63304c1e
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08916577B2

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