反応式
[CH2:1]([O:3][CH:4]([O:10][CH2:11][CH3:12])[C:5](OCC)=[O:6])[CH3:2].[OH-].[NH4+:14]>C(Cl)Cl>[CH2:1]([O:3][CH:4]([O:10][CH2:11][CH3:12])[C:5]([NH2:14])=[O:6])[CH3:2]参加物
4
実験手順
A mixture of 24.85 g of ethyl diethoxyacetate and 140 ml of concentrated ammonium hydroxide was stirred for 3 hours. The ammonia and H2O were evaporated under reduced pressure on a water bath at 50°-60° leaving a wet solid. The wet solid was dried in a vacuum oven at 53° for 18 hours giving a dark pink solid. The solid was dissolved in CH2Cl2. The solution was filtered to remove a small amount of red insoluble material. The filtrate was concentrated and Skellysolve B was added. Cooling gave 18.0 g (87%) of diethoxyacetamide as orange plates, m.p. 76.5-79°.
後処理
- customThe ammonia and H2O were evaporated under reduced pressure on a water bath at 50°-60°
- customleaving a wet solid
- customThe wet solid was dried in a vacuum oven at 53° for 18 hours
- customgiving a dark pink solid
- filtrationThe solution was filtered
- customto remove a small amount of red insoluble material
- concentrationThe filtrate was concentrated
- additionSkellysolve B was added
- temperatureCooling
出典と根拠
- ORDレコード
- ord-a2f03c228cfc4a80915bffdae99800be
- 出典データセット
- uspto-grants-1993_09
- 特許番号
- US05245046
関連ノート
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