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

HRID 370746노트

반응식

HRID 370746 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3fddfb3bb0af460ab14b8550a51723cd
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528311

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