Government regulation → 5-溴-4-氟水杨酸

HRID 17518笔记

反应方程式

HRID 17518 反应方程式
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([OH:11])[CH:3]=1.[Br:12]Br>C(O)(=O)C>[Br:12][C:10]1[C:2]([F:1])=[CH:3][C:4]([OH:11])=[C:5]([CH:9]=1)[C:6]([OH:8])=[O:7]

参与物

4

反应物 2

HCID 24408Government regulationHCID 676614-氟水杨酸

产物 1

HCID 184681915-溴-4-氟水杨酸收率 93%

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂2 次

反应条件

温度
60 °C

实验过程

4-Fluoro-2-hydroxybenzoic acid (29.01 g, 0.186 mol) was dissolved in acetic acid (290 ml), then a solution of bromine (31.18 g, 0.195 mol) dissolved in acetic acid (15 ml) was gradually dropwise added at room temperature (1 hour). After stirred at 60° C. for 24 hours, this was cooled to room temperature. The reaction liquid was dried to solidness under reduced pressure, the residue was dissolved in methanol (100 ml), and this was poured into water (600 ml). After stirring at room temperature for 15 minutes, the precipitated crystal was washed and collected by filtration, and dried to obtain the entitled compound (35.36 g, 93%) as a colorless solid.

后处理

  1. additionwas gradually dropwise added at room temperature (1 hour)
  2. temperaturethis was cooled to room temperature
  3. customThe reaction liquid
  4. customwas dried to solidness under reduced pressure
  5. dissolutionthe residue was dissolved in methanol (100 ml)
  6. additionthis was poured into water (600 ml)
  7. stirringAfter stirring at room temperature for 15 minutes
  8. washthe precipitated crystal was washed
  9. filtrationcollected by filtration
  10. customdried

来源与证据

ORD记录
ord-153440b1f9a7449d9fe9b96ed3eeff53
来源数据集
uspto-grants-2010_06
专利号
US07737166B2

反应笔记

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