반응식
[Mg].Cl[CH2:3][Si:4]([CH3:7])([CH3:6])[CH3:5].Cl[P:9]([N:15]([CH2:18][CH3:19])[CH2:16][CH3:17])[N:10]([CH2:13][CH3:14])[CH2:11][CH3:12]>BrCCBr.C(OCC)C>[CH2:18]([N:15]([P:9]([N:10]([CH2:11][CH3:12])[CH2:13][CH3:14])[CH2:3][Si:4]([CH3:7])([CH3:6])[CH3:5])[CH2:16][CH3:17])[CH3:19]참가 물질
반응 조건
- 온도
- -78 °C
실험 절차
In a 50 ml three-necked flask equipped with a dropping funnel and a magnetic stirrer, 0.36 g (14.8 mmol) of magnesium and 10 ml of anhydrous diethyl ether were charged at room temperature in a nitrogen gas atmosphere. After several drops of 1,2-dibromoethane were added so as to activate magnesium, 2.0 ml (14.2 mmol) of chloromethyltrimethylsilane were added dropwise carefully to avoid heat build-up. When the reaction solution was stirred for 1 hour while it was heated mildly with a drier, the solution darkened. Then, after the solution was cooled to −78° C., 3.0 g (14.2 mmol) of chlorobis(diethylamino)phosphine synthesized in (a) were added dropwise to the solution, and the resultant mixture was then returned to room temperature and refluxed for 1 hour. The resulting crystals were filtered off, washed with anhydrous diethyl ether, and purified by vacuum-distillation (0.2 kPa, 74.3-79.5° C.) to obtain 2.29 g of bis(diethylamino)(trimethylsilylmethyl)phosphine in the form of a colorless transparent liquid; the yield was 62%.
후처리
- customIn a 50 ml three-necked flask equipped with a dropping funnel and a magnetic stirrer
- additionwere added dropwise carefully
- temperatureto avoid heat
- temperaturewas heated mildly with a drier
- additionwere added dropwise to the solution
- customwas then returned to room temperature
- temperaturerefluxed for 1 hour
- filtrationThe resulting crystals were filtered off
- washwashed with anhydrous diethyl ether
- distillationpurified by vacuum-distillation (0.2 kPa, 74.3-79.5° C.)
출처 및 근거
- ORD 기록
- ord-3cf6c0ebd9604059b7c62efb57e53d67
- 출처 데이터셋
- uspto-grants-2014_10
- 특허 번호
- US08871974B2
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