반응식
[CH3:1][CH:2]([OH:8])[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7]>C(OC(=O)CCC)(=O)CCC>[C:2]([O:8][CH:2]([CH3:1])[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])(=[O:8])[CH2:3][CH2:4][CH3:5]참가 물질
3
실험 절차
Butyric anhydride (260 ml, Aldrich) was added to 2-heptanol (162 g, 1.4 mol, Aldrich) over a 1.5 hour period at 100-140° C. The mixture was heated to 160° for 4 hours. The reaction mixture was then cooled, washed with hot water, washed with aqueous sodium carbonate to remove butyric anhydride, dried over sodium sulfate, and then concentrated. Fractional distillation of the crude residue under vacuum provided 1-methylhexyl butyrate (85-110°/78-80 mm Hg, 85% yield), the structure of which was confirmed by mass spectroscopy, nuclear magnetic resonance spectroscopy, and infra red spectroscopy (not shown).
후처리
- temperatureThe mixture was heated to 160° for 4 hours
- temperatureThe reaction mixture was then cooled
- washwashed with hot water
- washwashed with aqueous sodium carbonate
- customto remove butyric anhydride
- dry with materialdried over sodium sulfate
- concentrationconcentrated
- distillationFractional distillation of the crude residue under vacuum
출처 및 근거
- ORD 기록
- ord-4635c16b95d14734bc4f70c31d9877c9
- 출처 데이터셋
- uspto-grants-1999_11
- 특허 번호
- US05993879
연결된 노트
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