Pyridine → Acetoxymethyl 2-methacryloyloxyethyl Carbonate

HRID 1900153ノート

反応式

HRID 1900153 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 23371997Acetoxymethyl 2-methacryloyloxyethyl Carbonate収率 65%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-fe29a4ad2aac47ca96e5083470ee6ca4
出典データセット
uspto-grants-1996_11
特許番号
US05574097

反応ノート

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