甲基硫酸酯-13C2 → 4-氨基-5-氯-2-羟基苯甲酸甲酯

HRID 5370

反应方程式

HRID 5370 反应方程式
[NH2:1][C:2]1[C:10]([Cl:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([OH:12])[CH:3]=1.C[O-].[Na+].CO.S(OC)(O[CH3:22])(=O)=O>CO.O>[NH2:1][C:2]1[C:10]([Cl:11])=[CH:9][C:5]([C:6]([O:8][CH3:22])=[O:7])=[C:4]([OH:12])[CH:3]=1

参与物

6

反应物 3

HCID 6497甲基硫酸酯-13C2HCID 148832224-氨基-5-氯-2-羟基苯甲酸HCID 23694274Sodium methanolate methanol

产物 1

HCID 148832234-氨基-5-氯-2-羟基苯甲酸甲酯收率 87%

试剂、催化剂与溶剂 2

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)-酮溶剂HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

A solution of 4-amino-5-chloro-2-hydroxybenzoic acid (1.88 g, 10 mmol) in absolute methanol (20 mL) was treated with 25% sodium methoxide/methanol (2.16 g, 10 mmol), stirred for 30 minutes, and concentrated in vacuo. The solid residue was taken up in anhydrous acetone (30 mL), treated with dimethyl sulfate (1.64 g, 13 mmol), and refluxed for 2 hours. The resultant solution was diluted with water (100 mL), and the precipitate was filtered, washed with water, and dried exhaustively in vacuo to afford 1.75 g (87%) of fine colorless needles. The material was recrystallized from ethyl acetate/hexane; mp 138°-139° C.

后处理

  1. concentrationconcentrated in vacuo
  2. temperaturerefluxed for 2 hours
  3. filtrationthe precipitate was filtered
  4. washwashed with water
  5. customdried exhaustively in vacuo

来源与证据

ORD记录
ord-5ef4854df60141d78ca949d2c8047a2b
来源数据集
uspto-grants-1993_09
专利号
US05244907

关联笔记

加载中…