Sodium Hydroxide → 2,2-Dimethyl-5-nitro-1,3-dioxane
反応式
[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]1参加物
4
反応条件
- 温度
- 60 °C
実験手順
Into a 250 ml round bottom flask equipped with a stir bar, thermometer and reflux condensor topped with a nitrogen inlet was added 5.73 g (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.
後処理
- customInto a 250 ml round bottom flask equipped with a stir bar
- temperaturethermometer and reflux condensor
- customtopped with a nitrogen inlet
- temperatureThe solution was cooled to 5° C. and at this temperature
- filtrationThe precipitated solid was filtered off
- customdried
出典と根拠
- ORDレコード
- ord-3ca6b5527b844164a0799330a60b4ad2
- 出典データセット
- uspto-grants-1989_07
- 特許番号
- US04851588
反応ノート
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