Ethyl Acetate → HCID 178449954、化合物

HRID 1268907ノート

反応式

HRID 1268907 の反応式
[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]

参加物

5

反応物 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

生成物 1

HCID 178449954HCID 178449954、化合物収率 61%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-2b52205fbad04097a3774891872b1814
出典データセット
uspto-grants-2007_04
特許番号
US07199137B2

反応ノート

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