Sodium Carbonate → Methyl 2-bromo-6-fluorobenzoate

HRID 1190926ノート

反応式

HRID 1190926 の反応式
[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4]([OH:6])=[O:5].[C:12](=O)([O-])[O-].[Na+].[Na+]>CO.S(=O)(=O)(O)O>[Br:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([F:11])[C:3]=1[C:4]([O:6][CH3:12])=[O:5]

参加物

5

反応物 2

HCID 10340Sodium CarbonateHCID 3026212-Bromo-6-fluorobenzoic acid

生成物 1

HCID 12192163Methyl 2-bromo-6-fluorobenzoate収率 85%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 1118Sulfuric Acid溶媒

反応条件

温度
80 °C

実験手順

2-Bromo-6-fluorobenzoic acid (1, 12.50 g, 57 mmol) was dissolved in a mixture of methanol (60 mL) and conc. sulfuric acid (65 mL). The solution was heated to 80° C. and stirred for 12 h. The reaction mixture was cooled and 20% sodium carbonate solution (500 mL) was added slowly to reach pH=8. The mixture was extracted with dichloromethane (3×180 mL), and the combined organic layers were dried over magnesium sulfate and evaporated. The title compound (11.29 g, 48.5 mmol, 85%) was obtained as a brown oil.

後処理

  1. temperatureThe reaction mixture was cooled
  2. extractionThe mixture was extracted with dichloromethane (3×180 mL)
  3. dry with materialthe combined organic layers were dried over magnesium sulfate
  4. customevaporated

出典と根拠

ORDレコード
ord-73cb7dbecb504f58b9a5a16cbe075a2a
出典データセット
uspto-grants-2014_03
特許番号
US08680099B2

反応ノート

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