Pyridine → HCID 86749865、化合物
反応式
Cl[C:2]([O:4][CH:5]([Cl:7])[CH3:6])=[O:3].[CH3:8][O:9][CH2:10][CH2:11]O.N1C=CC=CC=1>C(Cl)(Cl)Cl>[C:2](=[O:3])([OH:9])[OH:4].[Cl:7][CH:5]([CH2:11][CH2:10][O:9][CH3:8])[CH3:6]参加物
5
実験手順
1-Chloroethyl chloroformate (28.6 g, 0.2 mol) and 2-methoxyethanol (13.7 g, 0.18 mol) were dissolved in chloroform (220 ml) at 0° C. Pyridine (15.8 g, 0.2 mol) was added dropwise during 45 minutes maintaining the temperature below 12° C. After stirring at room temperature for 2 hours the mixture was washed three times with 1 normal hydrochloric acid, once with a saturated sodium hydrogen carbonate solution and finally twice with water. The organic phase was dried with magnesium sulfate and the solvent was removed at reduced pressure. The residue was distilled in vacuo. Yield: 75%. 1H-NMR: delta=1.76 (CHCH3); 3.27 (OCH3); 3.55 (CH2OCH3); 4.27 (COOCH2); 6.51 (CH).
後処理
- temperaturemaintaining the temperature below 12° C
- washwas washed three times with 1 normal hydrochloric acid
- dry with materialThe organic phase was dried with magnesium sulfate
- customthe solvent was removed at reduced pressure
- distillationThe residue was distilled in vacuo
出典と根拠
- ORDレコード
- ord-c9d92dde582746c7a2154814d3880154
- 出典データセット
- uspto-grants-1996_09
- 特許番号
- US05559266
反応ノート
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