Stannous chloride dihydrate → HCID 68665521、化合物

HRID 1893477ノート

反応式

HRID 1893477 の反応式
[Br:1][C:2]1[C:3]([C:16]([F:19])([F:18])[F:17])=[CH:4][C:5]([N+:13]([O-])=O)=[C:6]([N:8]2[CH:12]=[CH:11][N:10]=[CH:9]2)[CH:7]=1.O.O.Cl[Sn]Cl>C(O)C>[Br:1][C:2]1[C:3]([C:16]([F:19])([F:18])[F:17])=[CH:4][C:5]([NH2:13])=[C:6]([N:8]2[CH:12]=[CH:11][N:10]=[CH:9]2)[CH:7]=1

参加物

4

反応物 2

HCID 61436Stannous chloride dihydrateHCID 59333299HCID 59333299、化合物

生成物 1

HCID 68665521HCID 68665521、化合物収率 90%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1-[5-bromo-2-nitro-4-(trifluoromethyl)phenyl]-1H-imidazole (15.50 g, 0.0461 mol) is stirred with SnCl2.2H2O (51.77 g, 0.2274 mol) in ethanol (78 mL) at 80° C. for 2 hours. After cooling down to room temperature, the mixture is concentrated and partitioned between water (200 mL) and ethyl acetate (250 mL). Sodium hydrogencarbonate powder is added to adjust the pH to 8. The milky suspension is filtrated, the cake is washed with ethyl acetate and the combined organic phases are washed with water and dried over sodium sulfate. Concentration affords the title compound as a pale yellow solid (12.70 g, 90.0%)

後処理

  1. concentrationthe mixture is concentrated
  2. custompartitioned between water (200 mL) and ethyl acetate (250 mL)
  3. additionSodium hydrogencarbonate powder is added
  4. filtrationThe milky suspension is filtrated
  5. washthe cake is washed with ethyl acetate
  6. washthe combined organic phases are washed with water
  7. dry with materialdried over sodium sulfate
  8. concentrationConcentration

出典と根拠

ORDレコード
ord-00980ea6bfd44818a11b066a9c47bd8a
出典データセット
uspto-grants-2013_08
特許番号
US08513250B2

反応ノート

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