Ethyl Acetate → HCID 178449954, 화합물

HRID 1268907노트

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HRID 1268907 반응식
[NH2:1][CH2:2][C:3]([C:6]1[NH:7][C:8]([C:21]2[CH:26]=[CH:25][N:24]=[CH:23][CH:22]=2)=[C:9]([C:11]2[CH:12]=[C:13]3[C:17](=[CH:18][CH:19]=2)[C:16](=[O:20])[CH2:15][CH2:14]3)[N:10]=1)([CH3:5])[CH3:4].[CH3:27][S:28](Cl)(=[O:30])=[O:29].C(OCC)(=O)C>ClCCl>[CH3:4][C:3]([C:6]1[NH:10][C:9]([C:11]2[CH:12]=[C:13]3[C:17](=[CH:18][CH:19]=2)[C:16](=[O:20])[CH2:15][CH2:14]3)=[C:8]([C:21]2[CH:22]=[CH:23][N:24]=[CH:25][CH:26]=2)[N:7]=1)([CH3:5])[CH2:2][NH:1][S:28]([CH3:27])(=[O:30])=[O:29]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 31297Methanesulfonyl chlorideHCID 184469145-[2-(2-Amino-1,1-dimethyl-ethyl)-5-pyridin-4-yl-1H-imidazol-4-yl]-indan-1-one

생성물 1

HCID 178449954HCID 178449954, 화합물수율 61%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of the product of Example 1, Step 6 (0.1 g, 0.29 mmol) and methane sulphonyl chloride (0.023 ml, 0.3 mmol) in dichloromethane (3 ml) was stirred at room temperature for 2 hours. The reaction was then poured into ethyl acetate, washed with water and aqueous sodium hydrogen carbonate solution, dried (MgSO4) and concentrated in vacuo. The crude residue was then purified by silica gel chromatography eluting with a 1:9:90 mixture of 0.88 ammonia solution:methanol:dichloromethane to give the title compound (0.075 g, 61%) as a yellow solid; MS(AP+) m/e 425 [M+H]+.

후처리

  1. washwashed with water and aqueous sodium hydrogen carbonate solution
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. customThe crude residue was then purified by silica gel chromatography
  5. washeluting with a 1:9:90 mixture of 0.88 ammonia solution

출처 및 근거

ORD 기록
ord-2b52205fbad04097a3774891872b1814
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199137B2

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