Diethyl Ether → AlH(CH2CH2CH2NMe2)2
반응식
[AlH3:1].[N:2]([CH3:6])([CH3:5])[CH2:3][CH3:4].[Li][CH2:8][CH2:9][CH2:10][N:11]([CH3:13])[CH3:12].[CH2:14](OCC)C>>[AlH:1]([CH2:8][CH2:9][CH2:10][N:11]([CH3:13])[CH3:12])[CH2:14][CH2:4][CH2:3][N:2]([CH3:6])[CH3:5]참가 물질
5
반응 조건
- 온도
- -70 °C
실험 절차
A dried flask is charged with AlH3.NEtMe2 (6.60 g, 64 mmol) under an inert atmosphere (e.g., argon) and then 50 mL of diethyl ether. The resulting slurry is cooled to −70° C. and a solution of LiCH2CH2CH2NMe2 (260 mL of 0.5 M solution in diethyl ether) is added. The resulting mixture is allowed to warm slowly to room temperature and stirred for 18 hours. The solvent is then removed in vacuo and the crude product is transferred to a smaller distillation apparatus for purification by distillation under vacuum.
후처리
- temperatureto warm slowly to room temperature
- customThe solvent is then removed in vacuo
- distillationthe crude product is transferred to a smaller distillation apparatus for purification by distillation under vacuum
출처 및 근거
- ORD 기록
- ord-b14a1194f1374959a711274ee62c8030
- 출처 데이터셋
- uspto-grants-2005_12
- 특허 번호
- US06979370B2
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