1-Butanol → Diphenyl carbonate

HRID 565082노트

반응식

HRID 565082 반응식
[C:1]1([OH:7])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:8](=[O:19])([O:14][CH2:15][CH2:16][CH2:17][CH3:18])OCCCC.[CH2:20](O)[CH2:21]CC>>[C:8](=[O:19])([O:14][C:15]1[CH:16]=[CH:17][CH:18]=[CH:21][CH:20]=1)[O:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

4

반응물 3

HCID 2631-ButanolHCID 996Phenol2회HCID 68333Dibutyl carbonate2회

생성물 1

HCID 7597Diphenyl carbonate

실험 절차

After 150 minutes of starting of the reaction, the reflux ratio was set to 0.2 and unreacted phenol and dibutyl carbonate were mainly distilled out in a reflux ratio of 0.2 by lowering gradually the reaction pressure from atmospheric pressure to 450 mmHg. After 40 minutes, unreacted phenol and dibutyl carbonate were almost distilled out. At this time, the bottom section temperature was 205° C. Then, dibutyl carbonate due to disproportionation was mainly distilled out by further lowering gradually the reaction pressure to 100 mmHg. After 2 hours of setting the reflux ratio to 0.2, the reaction was completed. At this time, the reaction liquid was analyzed. At this time, the bottom section temperature was 207° C. The distilled-out liquid contained 668 g of dibutyl carbonate, 774 g of phenol and 18 g of butanol. The bottom liquid was further distilled in order to remove the catalyst, whereby 133 g of diphenyl carbonate was obtained as the distillate.

후처리

  1. customAfter 150 minutes of starting of the reaction
  2. distillationwere mainly distilled out in a reflux ratio of 0.2
  3. customthe reaction pressure from atmospheric pressure to 450 mmHg
  4. distillationunreacted phenol and dibutyl carbonate were almost distilled out
  5. customwas 205° C
  6. distillationThen, dibutyl carbonate due to disproportionation was mainly distilled out
  7. customthe reaction pressure to 100 mmHg
  8. waitAfter 2 hours of setting
  9. customAt this time, the reaction liquid
  10. customwas 207° C
  11. distillationThe bottom liquid was further distilled in order
  12. customto remove the catalyst

출처 및 근거

ORD 기록
ord-28a2097113f44c2f91167a8ad67c4dbc
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06169197A

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