Pyridine → Acetoxymethyl 2-methacryloyloxyethyl Carbonate

HRID 1900153노트

반응식

HRID 1900153 반응식
Cl[C:2]([O:4][CH2:5][O:6][C:7](=[O:9])[CH3:8])=[O:3].[C:10]([O:15][CH2:16][CH2:17][OH:18])(=[O:14])[C:11]([CH3:13])=[CH2:12].N1C=CC=CC=1>C(Cl)Cl>[C:2](=[O:3])([O:18][CH2:17][CH2:16][O:15][C:10](=[O:14])[C:11]([CH3:13])=[CH2:12])[O:4][CH2:5][O:6][C:7](=[O:9])[CH3:8]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 133602-Hydroxyethyl MethacrylateHCID 14800978[(Chlorocarbonyl)oxy]methyl acetate

생성물 1

HCID 23371997Acetoxymethyl 2-methacryloyloxyethyl Carbonate수율 65%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of acetoxymethyl chloroformate (1.00 g, 0.0066 mol) and 2-hydroxyethyl methacrylate (0.86 g, 0.0066 mol) in methylene chloride (30 ml), pyridine (0.52 g, 0.0066 mol) was added at 0° C. After 10 min at 0° C. and 18 hours at 25° C. the reaction mixture was washed with aqueous hydrochloric acid (100 ml), aqueous saturated sodium hydrogen carbonate (100 ml) and water (100 ml). The solvent was removed under reduced pressure after drying (MgSO4). Flash chromatography (silicagel, hexane/ethyl acetate (3:2)) gave 1.05 g (65%) of the title product.

후처리

  1. wash18 hours at 25° C. the reaction mixture was washed with aqueous hydrochloric acid (100 ml), aqueous saturated sodium hydrogen carbonate (100 ml) and water (100 ml)
  2. customThe solvent was removed under reduced pressure
  3. dry with materialafter drying (MgSO4)

출처 및 근거

ORD 기록
ord-fe29a4ad2aac47ca96e5083470ee6ca4
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05574097

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