反応式
Cl[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[O-:8][CH2:9][CH3:10].[Na+]>C(O)C>[CH2:9]([O:8][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH3:10]参加物
4
実験手順
A solution of ethyl chloracetate (100 g, 99% pure, 0.81 mol) in ethanol is treated with ethanolic sodium ethoxide (282.9 g, 20.6% solution, 0.86 mole NaOC2H5) over a 1 hr period at 20° C.-30° C., heated at 40° C.-45° C. for 0.5 hr, cooled to room temperature, treated with diatomaceous earth, stirred for 0.25 hr and filtered. The filtercake is washed with ethanol. The combined filtrates are distilled to obtain the title product as a colorless liquid 75.78 g, 98.8% pure (71% yield), bp 87° C.-88° C./59 mmHg, identified by 13CNMR, 1HNMR and mass spectral analyses.
後処理
- temperatureheated at 40° C.-45° C. for 0.5 hr
- additiontreated with diatomaceous earth
- filtrationfiltered
- washThe filtercake is washed with ethanol
- distillationThe combined filtrates are distilled
出典と根拠
- ORDレコード
- ord-bf0c80d3ebdd46919339dbf745980f16
- 出典データセット
- uspto-grants-1999_07
- 特許番号
- US05925764
関連ノート
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