Dimethylformamide → 5-benzyloxy-6-(2-fluorophenoxy)-2-pyrazin-2-yl-1H-benzimidazole

HRID 13327

反応式

HRID 13327 の反応式
O.O.[Sn](Cl)Cl.CN(C)C=O.[CH2:11]([O:18][C:19]1[C:24]([O:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[F:32])=[CH:23][C:22]([NH:33][C:34]([C:36]2[CH:41]=[N:40][CH:39]=[CH:38][N:37]=2)=O)=[C:21]([N+:42]([O-])=O)[CH:20]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C(OCC)(=O)C>[CH2:11]([O:18][C:19]1[C:24]([O:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=2[F:32])=[CH:23][C:22]2[NH:33][C:34]([C:36]3[CH:41]=[N:40][CH:39]=[CH:38][N:37]=3)=[N:42][C:21]=2[CH:20]=1)[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 61436Stannous chloride dihydrateHCID 23145658N-(4-benzyloxy-5-(2-fluorophenoxy)-2-nitrophenyl)pyrazinecarboxamide

生成物 1

HCID 231455135-benzyloxy-6-(2-fluorophenoxy)-2-pyrazin-2-yl-1H-benzimidazole

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

3.72 g of tin(II) chloride dihydrate was added to a dimethylformamide (16 ml) suspension of 1.52 g of N-(4-benzyloxy-5-(2-fluorophenoxy)-2-nitrophenyl)pyrazinecarboxamide, and the reaction liquid was stirred overnight at 80° C. The reaction liquid was diluted with ethyl acetate, washed with aqueous saturated sodium bicarbonate, water and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was washed with a mixed solvent of ethyl acetate and hexane to obtain the entitled compound as a yellow solid.

後処理

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. washwashed with aqueous saturated sodium bicarbonate, water and saturated saline in order
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. washthe resulting residue was washed with a mixed solvent of ethyl acetate and hexane

出典と根拠

ORDレコード
ord-2f53b352f3654eb7b81ad112302344a4
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

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