Azane;hydrate → 3-Chloro-4,5-dipropargyloxybenzamide
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([O:15][CH2:16][C:17]#[CH:18])[C:10]=1[O:11][CH2:12][C:13]#[CH:14])[C:5](Cl)=[O:6].O.[NH3:20]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:3]=[C:4]([CH:8]=[C:9]([O:15][CH2:16][C:17]#[CH:18])[C:10]=1[O:11][CH2:12][C:13]#[CH:14])[C:5]([NH2:20])=[O:6]参加物
4
実験手順
A solution of 3-choro-4,5-dipropargyloxybenzoyl chloride (1.00 g) in 30% ammonia water (20 ml) and toluene (10 ml) was stirred under reflux for 10 minutes, poured into ice-water and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate and concentrated under reduced pressure to give a residue. The residue was further washed with hexane to give 3-chloro-4,5-dipropargyloxybenzamide (0.88 g). m.p. 122°-125° C.
後処理
- temperatureunder reflux for 10 minutes
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under reduced pressure
- customto give a residue
- washThe residue was further washed with hexane
出典と根拠
- ORDレコード
- ord-a7b64744d83d465cb79c24a9e649dbed
- 出典データセット
- uspto-grants-1990_08
- 特許番号
- US04946865
反応ノート
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