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

HRID 13327노트

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HRID 13327 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2f53b352f3654eb7b81ad112302344a4
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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