Methanol → 5-Bromo-2-hydroxy-3-methylbenzoic acid

HRID 391443

反応式

HRID 391443 の反応式
[OH:1][C:2]1[C:10]([CH3:11])=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[Br:12]Br.O.CO>C(O)(=O)C>[Br:12][C:8]1[CH:9]=[C:10]([CH3:11])[C:2]([OH:1])=[C:3]([CH:7]=1)[C:4]([OH:6])=[O:5]

参加物

6

反応物 4

HCID 887Methanol2 回HCID 962WaterHCID 67383-Methylsalicylic AcidHCID 24408Bromine

生成物 1

HCID 27643455-Bromo-2-hydroxy-3-methylbenzoic acid

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

To a mixture of 2-hydroxy-3-methylbenzoic acid (2.1 g, 13.5 mmol) in acetic acid (30 mL) was added bromine (0.7 mL, 13.7 mmol) slowly over 5 minutes. After 24 h, water was added slowly to the reaction mixture and the reaction stirred for 30 min. The resulting precipitate was collected by filtration and washed several times with water. The product was dried overnight under high vacuum to afford 2.8 g (90%). LC/MS: tR=2.86 min, 229.14 (MH)+. (Phenomenex C18 4.6×50 mm, 10% MeOH/90% H2O/0.1% TFA→90% MeOH/10% H2O/0.1% TFA, Gradient time=4 min., Flow rate=4 mL/min.).

後処理

  1. filtrationThe resulting precipitate was collected by filtration
  2. washwashed several times with water
  3. customThe product was dried overnight under high vacuum
  4. customto afford 2.8 g (90%)

出典と根拠

ORDレコード
ord-c43b7d30147e43818ccab92c88f481e1
出典データセット
uspto-grants-2013_02
特許番号
US08383821B2

関連ノート

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