반응식
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]참가 물질
4
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-bf0c80d3ebdd46919339dbf745980f16
- 출처 데이터셋
- uspto-grants-1999_07
- 특허 번호
- US05925764
연결된 노트
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