Triethylamine → 2-(2'-Hydroxy-5'-methyacrylyloxypropyl-3'-tert-butylphenyl)-5-chloro-2H-benzotriazole

HRID 370746ノート

反応式

HRID 370746 の反応式
[C:1](Cl)(=[O:5])[C:2](C)=[CH2:3].[CH2:7](N(CC)CC)C.[OH:14][C:15]1[C:20]([C:21]([CH3:24])([CH3:23])[CH3:22])=[CH:19][C:18]([CH2:25][CH2:26][CH2:27][OH:28])=[CH:17][C:16]=1[N:29]1[N:33]=[C:32]2[CH:34]=[CH:35][C:36]([Cl:38])=[CH:37][C:31]2=[N:30]1>C(Cl)Cl>[OH:14][C:15]1[C:20]([C:21]([CH3:23])([CH3:22])[CH3:24])=[CH:19][C:18]([CH2:25][CH2:26][CH2:27][O:28][C:1](=[O:5])[CH:2]=[CH:3][CH3:7])=[CH:17][C:16]=1[N:29]1[N:33]=[C:32]2[CH:34]=[CH:35][C:36]([Cl:38])=[CH:37][C:31]2=[N:30]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 13528Methacryloyl chlorideHCID 136848972-(2'-hydroxy-5'-hydroxypropyl-3'-tert-butylphenyl)-5-chloro-2H-benzotriazole

生成物 1

HCID 765513612-(2'-Hydroxy-5'-methyacrylyloxypropyl-3'-tert-butylphenyl)-5-chloro-2H-benzotriazole

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

Methacrylyl chloride (5.9 ml) and triethylamine (8.5 ml) were added dropwise at -5° C. to a solution of 2-(2'-hydroxy-5'-hydroxypropyl-3'-tert-butylphenyl)-5-chloro-2H-benzotriazole (20 g) in 250 ml of methylene chloride. The reaction mixture was stirred at 0° C. overnight and then washed with 1N hydrochloric acid and water. The methylene chloride solution of the product was dried with sodium sulfate, passed through alumina column and evaporated. The crude yield of the product was 22 g (90%). A polymerization grade sample was obtained by recrystallization from methanol--methylene chloride mixture, m.p. 74.5°-76.5° C.

後処理

  1. washwashed with 1N hydrochloric acid and water
  2. dry with materialThe methylene chloride solution of the product was dried with sodium sulfate
  3. customevaporated
  4. customA polymerization grade sample was obtained by recrystallization from methanol

出典と根拠

ORDレコード
ord-3fddfb3bb0af460ab14b8550a51723cd
出典データセット
uspto-grants-1985_07
特許番号
US04528311

反応ノート

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