Morpholine → Acryloylmorpholine
반응식
[NH:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[C:14](Cl)(=[O:17])[CH:15]=[CH2:16]>C(OCC)C>[O:17]=[C:14]([N:1]1[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1)[CH:15]=[CH2:16]참가 물질
5
실험 절차
A solution of morpholine (8.7 g, 0.1 mole) and triethylamine (15.3 ml, 0.1 mole) in ethyl ether (100 ml) was cooled to +5° C. A solution of acryloyl chloride (9.0 g, 0.10 mole) in 25 ml of ethyl ether was added dropwise over a 30 minute period, resulting in the formation of a white solid. An additional 100 ml of ethyl ether was added and the reaction stirred for 72 hours at room temperature. The white solid was filtered and washed well with ethyl ether. The ethyl ether wash and filtrate were combined and solvent removed, leaving an orange oil which was transferred to a 50 ml Erlenmeyer flask and dried overnight under nitrogen to yield 11.5 g of product. The structure was confirmed by NMR.
후처리
- customresulting in the formation of a white solid
- filtrationThe white solid was filtered
- washwashed well with ethyl ether
- washThe ethyl ether wash
- customsolvent removed
- customleaving an orange oil which
- customdried overnight under nitrogen
출처 및 근거
- ORD 기록
- ord-689cdc64b5f44d938f8adf18839cf68b
- 출처 데이터셋
- uspto-grants-1991_01
- 특허 번호
- US04981853
반응 노트
불러오는 중…