Ammonia → 3-Amino-3-cyclopropyl-acrylic acid ethyl ester

HRID 129939ノート

反応式

HRID 129939 の反応式
C1(C)C=CC(S(O)(=O)=O)=CC=1.[CH:12]1([C:15]([CH2:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])=O)[CH2:14][CH2:13]1.[NH3:23].O>C1(C)C=CC=CC=1>[NH2:23][C:15]([CH:12]1[CH2:14][CH2:13]1)=[CH:17][C:18]([O:20][CH2:21][CH3:22])=[O:19]

参加物

6

反応物 4

HCID 222Ammonia2 回HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 262979Ethyl 3-cyclopropyl-3-oxopropanoate

生成物 1

HCID 534018893-Amino-3-cyclopropyl-acrylic acid ethyl ester

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

1.1 g of p-toluenesulphonic acid are added to 49.9 g (0.32 mol) of ethyl cyclopropylcarbonylacetate in 200 ml of dry toluene and the mixture is saturated with ammonia gas at room temperature with stirring. After allowing to stand overnight, the mixture is boiled under reflux for 8 hours in a water separator, ammonia gas being continuously introduced. The mixture is allowed to cool overnight and is filtered, and the toluene solution is concentrated in vacuo and removed by distillation in a high vacuum up to 65° C. from unreacted starting material. The substance is subsequently found in the residue. Yield: 11.9 g (24% of theory).

後処理

  1. additioncontinuously introduced
  2. temperatureto cool overnight
  3. filtrationis filtered
  4. concentrationthe toluene solution is concentrated in vacuo
  5. customremoved by distillation in a high vacuum up to 65° C.

出典と根拠

ORDレコード
ord-09c1f3d2568542a190722634d4ddee8b
出典データセット
uspto-grants-1995_11
特許番号
US05470982

反応ノート

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