Potassium Carbonate → HCID 17842074、化合物
反応式
[CH:1]1([C:5]([C:7]2[CH:12]=[CH:11][C:10]([O:13][CH3:14])=[CH:9][CH:8]=2)=O)[CH2:4][CH2:3][CH2:2]1.O.NN.C([O-])([O-])=O.[K+].[K+]>C(O)COCCO>[CH:1]1([CH2:5][C:7]2[CH:8]=[CH:9][C:10]([O:13][CH3:14])=[CH:11][CH:12]=2)[CH2:2][CH2:3][CH2:4]1参加物
5
実験手順
A mixture of compound (G) (5.00 g), hydrazine hydrate (4.12 g), K2CO3 (7.00 g) and diethylene glycol (16 ml) were heated to reflux temperature for 1 hour. The condenser was exchanged by a distillation device and the mixture was distilled at 220-230° C. The distillate was extracted with MTBE and the organic phase washed with water and brine, dried (MgSO4) and concentrated in vacuo. The residue was purified by chromatography to yield a colorless oil (4.4 g).
後処理
- temperaturewere heated
- temperatureto reflux temperature for 1 hour
- distillationthe mixture was distilled at 220-230° C
- extractionThe distillate was extracted with MTBE
- washthe organic phase washed with water and brine
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe residue was purified by chromatography
出典と根拠
- ORDレコード
- ord-5303ce8b359346df922f13f96f7808d8
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07704942B2
反応ノート
読み込み中…