3-羟基-2-氨基苯甲酸 → 2-Amino-5-bromo-3-hydroxybenzoic Acid

HRID 17512笔记

反应方程式

HRID 17512 反应方程式
[OH:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:4]([C:5]([OH:7])=[O:6])[C:3]=1[NH2:11].[Br:12]Br.CO.O>C(O)(=O)C>[NH2:11][C:3]1[C:2]([OH:1])=[CH:10][C:9]([Br:12])=[CH:8][C:4]=1[C:5]([OH:7])=[O:6]

参与物

6

反应物 4

HCID 863-羟基-2-氨基苯甲酸HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]HCID 24408Government regulation

产物 1

HCID 217551432-Amino-5-bromo-3-hydroxybenzoic Acid收率 97%

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂2 次

实验过程

3-Hydroxyanthranilic acid (6.28 g, 41.0 mmol) was dissolved in acetic acid (550 ml), then a solution of bromine (13.1 g, 82.0 mmol) dissolved in acetic acid (50 ml) was gradually and dropwise added at room temperature, taking 20 minutes. After stirring at room temperature for 2.5 hours, methanol (70 ml) and water (300 ml) were added to the solution, followed by stirring at room temperature for 15 hours. The formed solid was collected by nitration, and dried under reduced pressure to obtain the entitled compound (9.129 g, 97%) as a brown powder.

后处理

  1. additiondropwise added at room temperature
  2. stirringby stirring at room temperature for 15 hours
  3. customThe formed solid was collected by nitration
  4. customdried under reduced pressure

来源与证据

ORD记录
ord-4ad1f4d15d514ec0aa6dbe5e8378817a
来源数据集
uspto-grants-2010_06
专利号
US07737166B2

反应笔记

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