Phosphorus trichloride → HCID 178522602、化合物

HRID 2301412ノート

反応式

HRID 2301412 の反応式
[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

参加物

5

反応物 3

HCID 24387Phosphorus trichlorideHCID 145347685-Bromo-8-hydroxyquinoline-7-carboxylic acidHCID 183727262-Amino-5-(4-chlorophenyl)-4-thiazolol

生成物 1

HCID 178522602HCID 178522602、化合物収率 11.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c9c5a140e83f4502babcfdf01816369b
出典データセット
uspto-grants-2002_12
特許番号
US06500842B1

反応ノート

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