巯基乙胺 → 2-(2-Chloro-5-pyridyl)thiazolidine

HRID 22223

反应方程式

HRID 22223 反应方程式
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[CH:4][N:3]=1.[NH2:10][CH2:11][CH2:12][SH:13]>C1C=CC=CC=1>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]2[NH:10][CH2:11][CH2:12][S:13]2)=[CH:4][N:3]=1

参与物

4

反应物 2

HCID 6058巯基乙胺HCID 27640536-氯烟醛

产物 1

HCID 137527892-(2-Chloro-5-pyridyl)thiazolidine收率 89.9%

试剂、催化剂与溶剂 1

HCID 241苯溶剂

实验过程

A solution composed of 6-chloronicotinaldehyde (14.2 g), 2-aminoethanethiol (7.7 g) and benzene (80 ml) was heated with stirring for 5 hours while removing water as an azeotrope. After the reaction, benzene was distilled off under reduced pressure, and further volatile materials were removed at 1 mmHg and 70° C. to give 2-(2-chloro-5-pyridyl)thiazolidine (18 g) as a residue. Ten grams of 2-(2-chloro-5-pyridyl)thiazolidine was dissolved in 100 ml of ethanol, and sodium borohydride was added. With stirring, the mixture was gradually heated and thereafter refluxed for 1 hour. Ethanol was distilled off under reduced pressure, and chloroform was added to the residue. Insoluble materials were separated by filtration and the chloroform layer was washed with water and dehydrated. Chloroform was distilled off under reduced pressure to give the desired N-(2-chloro-5-pyridylmethyl)2-aminoethanethiol (8.3 g).

后处理

  1. temperaturewas heated
  2. customwhile removing water as an azeotrope
  3. customAfter the reaction, benzene
  4. distillationwas distilled off under reduced pressure, and further volatile materials
  5. customwere removed at 1 mmHg and 70° C.

来源与证据

ORD记录
ord-55ad2e916fc14fdc96af4991eedb5385
来源数据集
uspto-grants-1995_06
专利号
US05428032

关联笔记

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