반응식
[C:1](=[O:8])([O:3][CH2:4][CH2:5][CH2:6][CH3:7])N.[C:9]1([OH:15])C=C[CH:12]=[CH:11][CH:10]=1>>[C:1](=[O:8])([O:15][CH2:9][CH2:10][CH2:11][CH3:12])[O:3][CH2:4][CH2:5][CH2:6][CH3:7]참가 물질
실험 절차
A liquid containing 42.6% by weight (hereinafter, “wt %”) of dibutyl carbonate, 11.4 wt % of butyl carbamate and 46.0 wt % of phenol was fed at the rate of 300 g/hr at 100° C. to a center portion of a distillation column made from glass provided with a vacuum jacket (filled Sulzer Labopacking, inner diameter 50 mmφ, height of filling portion: concentration portion 550 mm, recovery portion 550 mm) and the continuous distillation was performed under a top section pressure of 20 mmHg in the distillation column. The distillation column was operated in a reflux ratio of 3 and adjusted to distill out 265 g/hr of a distillate from the top section and thus steady state was maintained. In the distillation, a liquid containing 48.2 wt % of dibutyl carbonate and 51.8 wt % of phenol was obtained as a distillate of the top section. Butyl carbamate content in the liquid thus obtained was below 0.05 wt %. A liquid containing 98.0 wt % of butyl carbamate and 2.0 wt % of phenol was obtained at the rate of 35 g/hr from the bottom section. Dibutyl carbonate content in the liquid thus obtained was below 0.05 wt %. In this distillation, the top section temperature was 94° C. and the bottom section temperature was 118° C.
후처리
- customwas obtained at the rate of 35 g/hr from the bottom section
출처 및 근거
- ORD 기록
- ord-975ae0790927472186f2270556bd605d
- 출처 데이터셋
- uspto-grants-2001_01
- 특허 번호
- US06169197A
연결된 노트
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