Sodium Hydroxide → 2,2-Dimethyl-5-nitro-1,3-dioxane
반응식
[CH3:1][C:2]1([CH3:13])[O:7][CH2:6][C:5](CO)([N+:8]([O-:10])=[O:9])[CH2:4][O:3]1.[OH-].[Na+]>C(O)(=O)C>[CH3:1][C:2]1([CH3:13])[O:3][CH2:4][CH:5]([N+:8]([O-:10])=[O:9])[CH2:6][O:7]1참가 물질
4
반응 조건
- 온도
- 60 °C
실험 절차
Into a 250 ml round bottom flask equipped with a stir bar, thermometer and reflux condenser topped with a nitrogen inlet was added 5.73 (0.03) mole) of 2,2-dimethyl-5-hydroxymethyl-5-nitro-1,3-dioxane and 70 ml 10% sodium hydroxide which was heated to 60° C. for one hour. The solution was cooled to 5° C. and at this temperature acidified to pH 5 with concentrated acetic acid. The precipitated solid was filtered off and dried to give 5.2 g (92%) of 2,2-dimethyl-5-nitro-1,3-dioxane m.p. 60°-61° C. 1H NMR in CD3OD also confirmed the structure.
후처리
- customInto a 250 ml round bottom flask equipped with a stir bar
- temperaturethermometer and reflux condenser
- customtopped with a nitrogen inlet
- temperatureThe solution was cooled to 5° C. and at this temperature
- filtrationThe precipitated solid was filtered off
- customdried
출처 및 근거
- ORD 기록
- ord-db567f22b07c43468c490318f9d65adb
- 출처 데이터셋
- uspto-grants-1990_12
- 특허 번호
- US04978793
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