氯化亚砜 → 6-氯甲基吡啶-3-甲酸乙酯

HRID 2356616

反应方程式

HRID 2356616 反应方程式
S(Cl)([Cl:3])=O.O[CH2:6][C:7]1[N:12]=[C:11]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:10]=[CH:9][CH:8]=1>>[Cl:3][CH2:6][C:7]1[N:12]=[C:11]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:10]=[CH:9][CH:8]=1

参与物

3

反应物 2

HCID 24386氯化亚砜HCID 109211416-羟甲基吡啶-2-甲酸乙酯

产物 1

HCID 156140036-氯甲基吡啶-3-甲酸乙酯

反应条件

温度
12.5 °C

实验过程

Thionyl chloride (13.8 ml) was added over ˜15 minutes to a stirred solution of ethyl 6-(hydroxymethyl)-2-pyridinecarboxylate (28.5 g) in MDC (200 ml) maintaining the temperature at 10-15° C. using an ice-water bath. On completion of the addition the mixture was stirred at room temperature for 1 hour. The solvent was evaporated and the residue partitioned between toluene (200 ml)/saturated bicarb (sodium bicarbonate solution, 200 ml). The layers were separated and the organic phase washed with water (150 ml). The solvent was evaporated to leave a pale oil which solidified on standing. (31.3 g).

后处理

  1. additionOn completion of the addition the mixture
  2. customThe solvent was evaporated
  3. customthe residue partitioned between toluene (200 ml)/saturated bicarb (sodium bicarbonate solution, 200 ml)
  4. customThe layers were separated
  5. washthe organic phase washed with water (150 ml)
  6. customThe solvent was evaporated
  7. customto leave a pale oil which

来源与证据

ORD记录
ord-1df03204a7da44a6b0d601d75004ba84
来源数据集
uspto-grants-2010_07
专利号
US07759369B2

关联笔记

加载中…