HCID 90410240, 화합물 → 2-Amino-6-bromo-4-fluoro-3-nitrophenol

HRID 928552노트

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HRID 928552 반응식
[Br:1][C:2]1[C:7]([OH:8])=[C:6]([N+:9]([O-])=O)[C:5]([N+:12]([O-:14])=[O:13])=[C:4]([F:15])[CH:3]=1>CO.Cl.O>[NH2:9][C:6]1[C:5]([N+:12]([O-:14])=[O:13])=[C:4]([F:15])[CH:3]=[C:2]([Br:1])[C:7]=1[OH:8]

참가 물질

5

반응물 1

HCID 90410240HCID 90410240, 화합물

생성물 1

HCID 904098182-Amino-6-bromo-4-fluoro-3-nitrophenol

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 887Methanol용매HCID 962Water용매2회

실험 절차

To a stirred solution of 6-bromo-4-fluoro-2,3-dinitrophenol (4.4 g, 16 mmol) in methanol (88 mL) and 12.0 M hydrogen chloride in water (40 mL) was added stannous chloride, dihydrate (11 g, 47 mmol). The reaction was stirred at RT for 15 min. Water was added and the mixture was extracted with ethyl acetate. The organic layer was separated and concentrated. Purification on silica gel using ethyl acetate in hexanes gave the desired compound, 2.48 g, 63%. 1H NMR (300 MHz, DMSO-d6) δ 9.80 (br s, 3H), 6.80 (m, 1H).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. customThe organic layer was separated
  3. concentrationconcentrated
  4. customPurification on silica gel

출처 및 근거

ORD 기록
ord-948fb2490ca34717aa36d6b648892bfe
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290514B2

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