三氯化磷 → HCID 178522602，化合物

HRID 1069504笔记

反应方程式

HRID 1069504 反应方程式
[Br:1][C:2]1[CH:11]=[C:10]([C:12]([OH:14])=O)[C:9]([OH:15])=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[N:7]2.[NH2:16][C:17]1[S:18][C:19]([C:23]2[CH:28]=[CH:27][C:26]([Cl:29])=[CH:25][CH:24]=2)=[C:20]([OH:22])[N:21]=1.P(Cl)(Cl)Cl>O>[Br:1][C:2]1[CH:11]=[C:10]([C:12]([NH:16][C:17]2[S:18][CH:19]([C:23]3[CH:24]=[CH:25][C:26]([Cl:29])=[CH:27][CH:28]=3)[C:20](=[O:22])[N:21]=2)=[O:14])[C:9]([OH:15])=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[N:7]2

参与物

5

反应物 3

HCID 24387三氯化磷HCID 145347685-溴-8-羟基喹啉-7-羧酸HCID 183727262-Amino-5-(4-chlorophenyl)-4-thiazolol

产物 1

HCID 178522602HCID 178522602，化合物收率 11.5%

试剂、催化剂与溶剂 1

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 5-bromo-8-hydroxyquinoline-7-carboxylic acid (0.268 g) of Preparation 2 and 2-amino-5-(4-chlorophenyl)-4-hydroxy-1,3-thiazole (0.227 g) in 50 mL xylenes is heated to reflux. To this is added dropwise PCl3 (0.069 g). Refluxing is continued overnight. The reaction is then cooled and water is added to destroy excess PCl3. The resulting solid is collected, washed with water and dried. The crude product is recrystallized from HOAc to yield 0.055 g of the title product as an orange solid.

后处理

  1. temperatureis heated to reflux
  2. temperatureRefluxing
  3. temperatureThe reaction is then cooled
  4. customto destroy excess PCl3
  5. customThe resulting solid is collected
  6. washwashed with water
  7. customdried
  8. customThe crude product is recrystallized from HOAc

来源与证据

ORD记录
ord-44e0cd1d5ba2414b9017de336a3ad5be
来源数据集
uspto-grants-2001_06
专利号
US06252080B1

反应笔记

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