Iodine → 1,3-Dioxolane-2-propionaldehyde
反応式
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]参加物
6
実験手順
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)+.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-cb2e95cbfab14f60ac1af2e9fbf5e1e1
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08835475B2
反応ノート
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