Ammonium Hydroxide → 2,2-Diethoxyacetamide

HRID 5602

反応式

HRID 5602 の反応式
[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

  1. customThe ammonia and H2O were evaporated under reduced pressure on a water bath at 50°-60°
  2. customleaving a wet solid
  3. customThe wet solid was dried in a vacuum oven at 53° for 18 hours
  4. customgiving a dark pink solid
  5. filtrationThe solution was filtered
  6. customto remove a small amount of red insoluble material
  7. concentrationThe filtrate was concentrated
  8. additionSkellysolve B was added
  9. 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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