HCID 90410240、化合物 → 2-Amino-6-bromo-4-fluoro-3-nitrophenol

HRID 928552ノート

反応式

HRID 928552 の反応式
[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]

参加物

5

反応物 1

HCID 90410240HCID 90410240、化合物

生成物 1

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

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-948fb2490ca34717aa36d6b648892bfe
出典データセット
uspto-grants-2016_03
特許番号
US09290514B2

反応ノート

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