Sulfuric Acid → 2-Bromo-4-methoxy-6-nitrophenol

HRID 1247203ノート

反応式

HRID 1247203 の反応式
[Br:1]Br.[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[C:7]([N+:12]([O-:14])=[O:13])[CH:6]=1.C([O-])(=O)C.[Na+].S(=O)(=O)(O)O>C(O)(=O)C.O>[Br:1][C:9]1[CH:10]=[C:5]([O:4][CH3:3])[CH:6]=[C:7]([N+:12]([O-:14])=[O:13])[C:8]=1[OH:11]

参加物

7

反応物 4

HCID 1118Sulfuric AcidHCID 15285Phenol, 4-methoxy-2-nitro-HCID 24408BromineHCID 517045Sodium Acetate

生成物 1

HCID 112651402-Bromo-4-methoxy-6-nitrophenol

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 962Water溶媒

実験手順

Bromine (16.0 g, 100 mmol) in acetic acid (20 mL) was added into a mixture of 4-methoxy-2-nitrophenol (16.9 g, 100 mmol, sodium acetate (16.4 g, 200 mmol) and acetic acid (100 mL). The mixture was stirred for 30 min at room temperature, and then at 70° C. for 2 h and poured into water (1.5 l) containing concentrated sulfuric acid (10 mL). The precipitated solid filtered and crystallized from (chloroform/hexane) to give a brownish solid, m.p. 116–118° C.; MS m/e 246 (M−H)+.

後処理

  1. waitat 70° C. for 2 h
  2. filtrationThe precipitated solid filtered
  3. customcrystallized from (chloroform/hexane)
  4. customto give a brownish solid, m.p. 116–118° C.

出典と根拠

ORDレコード
ord-54c812a22c654d0d9d06587e3d78d7f8
出典データセット
uspto-grants-2006_10
特許番号
US07129258B2

反応ノート

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