Stannous chloride dihydrate → HCID 68665521, 화합물

HRID 1893477노트

반응식

HRID 1893477 반응식
[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

참가 물질

4

반응물 2

HCID 61436Stannous chloride dihydrateHCID 59333299HCID 59333299, 화합물

생성물 1

HCID 68665521HCID 68665521, 화합물수율 90%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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%)

후처리

  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

출처 및 근거

ORD 기록
ord-00980ea6bfd44818a11b066a9c47bd8a
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513250B2

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