Iodine → 1,3-Dioxolane-2-propionaldehyde
반응식
Br[CH2:2][CH2:3][CH:4]1[O:8][CH2:7][CH2:6][O:5]1.[Mg].II.CN([CH:15]=[O:16])C>C1COCC1>[O:5]1[CH2:6][CH2:7][O:8][CH:4]1[CH2:3][CH2:2][CH:15]=[O:16]참가 물질
6
실험 절차
To the solution of 2-(2-bromoethyl)-1,3-dioxolane (10 g, 55.2 mmol) in THF (50 mL) was added magnesium (1.6 g, 66.3 mmol) and trace amount of I2 as initiator. The reaction mixture was stirred at rt for 2 hrs. After cooling to −78° C., the mixture was quenched with dry DMF (1.39 g, 66.3 mmol) and kept at −78° C. for 2 hrs. After dilution with H2O the reaction mixture was extracted with CH2Cl2 (2×), followed by distillation (45-55° C. @ 8 mmHg) to afford 2 g (28%) of the title compound. MS (DCI/NH4+) m/z 131 (M+H)+.
후처리
- temperatureAfter cooling to −78° C.
- waitkept at −78° C. for 2 hrs
- extractionAfter dilution with H2O the reaction mixture was extracted with CH2Cl2 (2×)
- distillationfollowed by distillation (45-55° C. @ 8 mmHg)
출처 및 근거
- ORD 기록
- ord-cb2e95cbfab14f60ac1af2e9fbf5e1e1
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08835475B2
반응 노트
불러오는 중…