Thionyl Chloride → 4-[(2-Oxido-1,3,2-dioxathiolan-4-yl)methyl]morpholine hydrochloride
반응식
[N:1]1([CH2:7][CH:8]([OH:11])[CH2:9][OH:10])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.[S:12](Cl)([Cl:14])=[O:13]>C(Cl)Cl>[ClH:14].[O:13]=[S:12]1[O:11][CH:8]([CH2:7][N:1]2[CH2:6][CH2:5][O:4][CH2:3][CH2:2]2)[CH2:9][O:10]1참가 물질
4
반응 조건
- 온도
- 0 °C
실험 절차
3-Morpholin-4-ylpropane-1,2-diol (2.1 g, 9.07 mmol) was dissolved in DCM (15 mL) and cooled to 0° C. The cooled solution was treated with thionyl chloride (1.81 mL, 24.8 mmol) and then heated at the reflux temperature for 1 h. The reaction mixture was then concentrated under reduced pressure to give a solid (2.5 g, 97%): 1H NMR (DMSO-d6) δ: 11.4 (1H, br s), 5.64-5.55 (1H, m) 4.82 (1H, dd), 4.50 (1H, dd), 4.02-3.71 (4H, m), 3.55-3.33 (4H, m), 3.26-3.06 (2H, br s).
후처리
- temperatureheated at the reflux temperature for 1 h
- concentrationThe reaction mixture was then concentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-0922c837f9414467b8e51e61a03467f4
- 출처 데이터셋
- uspto-grants-2014_11
- 특허 번호
- US08895549B2
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