반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH:2]1[C:7]([NH2:9])=[O:8].C(=O)([O-])O.[Na+].[CH:15](I)([CH3:17])[CH3:16]>C(#N)C.ClCCl>[CH3:16][CH:15]([N:1]1[CH2:6][CH2:5][O:4][CH2:3][CH:2]1[C:7]([NH2:9])=[O:8])[CH3:17]참가 물질
6
반응 조건
- 온도
- 150 °C
실험 절차
To a solution of 1.1 g (6.3 mmol) of morpholine-3-carboxamide (a synthesis of which is described in WO-2005/026 156, Hennequin L. F. A. et al.) in acetonitrile (16 ml) are successively added 1.86 g (22.2 mmol) of sodium hydrogen carbonate powder and 0.7 ml (7.0 mmol) of isopropyl iodide, and the mixture is then heated at 150° C. by microwave for 30 minutes. The reaction mixture is cooled to room temperature, diluted with dichloromethane (30 ml) and filtered through Celite. The filtrate is concentrated under reduced pressure and 1.1 g of compound are obtained in the form of a beige-coloured powder, which is used without further purification in the following step. Yield: 97%. MH+: 173.2 (tr: 0.72 min., condition 1).
후처리
- temperatureThe reaction mixture is cooled to room temperature
- filtrationfiltered through Celite
- concentrationThe filtrate is concentrated under reduced pressure and 1.1 g of compound
- customare obtained in the form of a beige-coloured powder, which
- customis used without further purification in the following step
- custom173.2 (tr: 0.72 min., condition 1)
출처 및 근거
- ORD 기록
- ord-78e15b2011ae4b189ce1f236f24382e2
- 출처 데이터셋
- uspto-grants-2013_05
- 특허 번호
- US08436011B2
연결된 노트
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