三硫代碳酸钠 → Sodium (2-methyl-3-hydroxy-5-vinyl-4-pyridinyl)methyl trithiocarbonate

HRID 614424

反应方程式

HRID 614424 反应方程式
[CH3:1][C:2]1[C:7]([OH:8])=[C:6]([CH2:9]Cl)[C:5]([CH:11]=[CH2:12])=[CH:4][N:3]=1.[C:13](=[S:16])([S-:15])[S-:14].[Na+:17].[Na+]>O.CO>[C:13](=[S:14])([S-:16])[S:15][CH2:9][C:6]1[C:5]([CH:11]=[CH2:12])=[CH:4][N:3]=[C:2]([CH3:1])[C:7]=1[OH:8].[Na+:17]

参与物

4

反应物 2

HCID 101753三硫代碳酸钠HCID 202639602-Methyl-3-hydroxy-4-chloromethyl-5-vinylpyridine

产物 1

HCID 86736400Sodium (2-methyl-3-hydroxy-5-vinyl-4-pyridinyl)methyl trithiocarbonate

试剂、催化剂与溶剂 1

HCID 22242641Methanol--water (1/1)溶剂

反应条件

温度
50 °C

实验过程

2-Methyl-3-hydroxy-4-chloromethyl-5-vinylpyridine (20 g.) is suspended in water/methanol (100:25 v/v) and treated with disodium trithiocarbonate (33%) (45 g.). The mixture is stirred at b 50° C. for 4 hours under nitrogen and adjusted to pH 6.2-6.5 with dilute acid. The precipitate is recrystallized from DMF/water to give sodium (2-methyl-3-hydroxy-5-vinyl-4-pyridinyl)methyl trithiocarbonate.

后处理

  1. additionwith dilute acid
  2. customThe precipitate is recrystallized from DMF/water

来源与证据

ORD记录
ord-0a0bd7c9e6a84b43aa484dc988503ae7
来源数据集
uspto-grants-1979_03
专利号
US04144342

关联笔记

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