Morpholine → 4-(3-Butyn-1-yl)morpholine
반응식
[CH2:1](OS(C)(=O)=O)[CH2:2][C:3]#[CH:4].[NH:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1>CCOCC>[CH2:1]([N:10]1[CH2:15][CH2:14][O:13][CH2:12][CH2:11]1)[CH2:2][C:3]#[CH:4]참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
A mixture of methanesulfonic acid but-3-ynyl ester (10.1 g, 68 mmol) and morpholine (12.5 mL, 143 mmol) was heated to 100° C. for 1 h. The mixture was diluted with Et2O (50 mL) and filtered. The solid residue was discarded, and the mother liquor extracted with 3N HCl. The aqueous layer was basified with NaOH, and back-extracted into EtOAc. Drying (Na2SO4), concentration, and distillation (short-path, b.p.=130° C. at ˜5 mm Hg) gave the title compound as a colorless oil. 1H NMR (CDCl3) δ 3.72 (t, 4H), 2.60 (t, 2H), 2.48 (t, 4H), 2.39 (td, 2H), 2.00 (t, 1H).
후처리
- filtrationfiltered
- extractionthe mother liquor extracted with 3N HCl
- extractionback-extracted into EtOAc
- customDrying
- concentration(Na2SO4), concentration, and distillation (short-path, b.p.=130° C. at ˜5 mm Hg)
출처 및 근거
- ORD 기록
- ord-da27fac848e640bf84cbb2303b967525
- 출처 데이터셋
- uspto-grants-2009_06
- 특허 번호
- US07544672B2
반응 노트
불러오는 중…