Water → (1-Ethyl-1-methylpropyl)cyclopentadiene
반응식
[CH2:1]([C:3]([CH2:9][CH3:10])=[C:4]1[CH:8]=[CH:7][CH:6]=[CH:5]1)[CH3:2].[CH3:11][Li].O>CCOCC>[CH2:1]([C:3]([C:4]1[CH2:8][CH:7]=[CH:6][CH:5]=1)([CH3:11])[CH2:9][CH3:10])[CH3:2]참가 물질
5
실험 절차
To a solution of 8.00 g (59.6 mol) of 6,6-diethylfulvene in 35 ml of ether, 60.0 ml (68.4 mmol) of an ether solution of methyllithium was dropwise added in a nitrogen atmosphere with ice cooling, followed by stirring at room temperature for one night. Then, 30 ml of water was added. The separated organic phase was washed with water and a saturated saline solution, then dried over magnesium sulfate and filtered. From the filtrate, the solvent was removed under reduced pressure to obtain a liquid. The liquid was subjected to vacuum distillation (92° C./40 mmHg) to obtain 5.50 g (36.6 mmol) of a light yellow liquid (yield: 61%). The analyzed values are given below.
후처리
- washThe separated organic phase was washed with water
- dry with materiala saturated saline solution, then dried over magnesium sulfate
- filtrationfiltered
- customFrom the filtrate, the solvent was removed under reduced pressure
- customto obtain a liquid
- distillationThe liquid was subjected to vacuum distillation (92° C./40 mmHg)
출처 및 근거
- ORD 기록
- ord-039bb3abc6524254ac4735a3eaaa05f8
- 출처 데이터셋
- uspto-grants-2008_11
- 특허 번호
- US07449533B2
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