Carbon Dioxide → Dihexyl carbonate

HRID 2115594

반응식

HRID 2115594 반응식
[CH2:1]([O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])CCCCC.C([Sn]CCCC)CCC.[CH2:23]([OH:29])[CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].C(=O)=[O:31]>>[C:1](=[O:31])([O:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH3:13])[O:29][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]

참가 물질

4

반응물 3

HCID 280Carbon Dioxide4회HCID 81031-HexanolHCID 86597556Dibutyltin dihexyloxide

생성물 1

HCID 522576Dihexyl carbonate수율 18%

반응 조건

온도
30 °C

실험 절차

Into a 100-ml autoclave (manufactured and sold by Toyo Koatsu Co., Ltd., Japan) were charged about 2.2 g of an organometal compound containing about 5 mmol of dibutyltin dihexyloxide (wherein the organometal compound was contained in the above-obtained reaction mixture) and 25.5 g (250 mmol) of hexanol (manufactured and sold by Aldrich, U.S.A.; a dehydrated grade). The autoclave was sealed. Then, from a carbon dioxide gas bomb, carbon dioxide gas, the pressure of which was lowered to 4 MPa by means of a pressure regulator connected to the carbon dioxide gas bomb, was introduced into the autoclave. Stirring of the contents of the autoclave was started. 10 Minutes after the start of the stirring, the valve of the carbon dioxide gas bomb was closed. Then, the internal temperature of the autoclave was elevated to 120° C. while stirring. Thereafter, carbon dioxide gas was gradually withdrawn from the autoclave through a purge line so as to adjust the internal pressure of the autoclave to 4 MPa. Then, a reaction was performed for 100 hours while maintaining the internal pressure of the autoclave at 4 MPa. After that period, the inside of the autoclave was cooled to about 30° C., and the internal pressure of the autoclave was returned to atmospheric pressure by gently purging the carbon dioxide gas through a purge line, and there was obtained a transparent reaction mixture. In the reaction mixture, dihexyl carbonate was obtained in a yield of 18%.

후처리

  1. customThe autoclave was sealed
  2. additionwas introduced into the autoclave
  3. customwas elevated to 120° C.
  4. stirringwhile stirring
  5. customThereafter, carbon dioxide gas was gradually withdrawn from the autoclave through a purge line so as
  6. temperaturewhile maintaining the internal pressure of the autoclave at 4 MPa
  7. waitAfter that period
  8. customby gently purging the carbon dioxide gas through a purge line
  9. customthere was obtained a transparent reaction mixture

출처 및 근거

ORD 기록
ord-3bacffd4f56041cb965f042c4ce60137
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07435842B2

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