Methyl 4-amino-3-iodo-5-nitrobenzoate → Methyl 3,4-diamino-5-iodobenzoate

HRID 446226

반응식

HRID 446226 반응식
[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:9]=[C:8]([N+:10]([O-])=O)[C:7]([NH2:13])=[C:6]([I:14])[CH:5]=1>C(OCC)(=O)C>[CH3:1][O:2][C:3](=[O:15])[C:4]1[CH:5]=[C:6]([I:14])[C:7]([NH2:13])=[C:8]([NH2:10])[CH:9]=1

참가 물질

3

반응물 1

HCID 67512142Methyl 4-amino-3-iodo-5-nitrobenzoate

생성물 1

HCID 67512100Methyl 3,4-diamino-5-iodobenzoate

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
70 °C

실험 절차

To a solution of 4-amino-3-iodo-5-nitro-benzoic acid methyl ester in ethyl acetate (50 mL) was added SnCl2 dihydrate. The mixture was heated to 70° C. for two hours, then cooled to room temperature and partitioned between ethyl acetate and saturated aqueous sodium bicarbonate. The organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure to provide 1.68 g (quantitative) of 3,4-diamino-5-iodo-benzoic acid methyl ester.

후처리

  1. temperaturecooled to room temperature
  2. custompartitioned between ethyl acetate and saturated aqueous sodium bicarbonate
  3. customThe organic layer was separated
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-8b876b71f5914e3cb992a1c68db7bca0
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476457B2

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