Ammonia → Ethyl 3-amino-4-methyl-pent-2-enoate

HRID 36916

反応式

HRID 36916 の反応式
C1(C)C=CC(S(O)(=O)=O)=CC=1.O.[C:13]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])(=O)[CH:14]([CH3:16])[CH3:15].[NH3:24]>C1(C)C=CC=CC=1>[NH2:24][C:13]([CH:14]([CH3:16])[CH3:15])=[CH:18][C:19]([O:21][CH2:22][CH3:23])=[O:20]

参加物

6

反応物 4

HCID 222Ammonia2 回HCID 962Water3 回HCID 6101p-Toluenesulfonic acidHCID 81583Ethyl isobutyrylacetate

生成物 1

HCID 59557418Ethyl 3-amino-4-methyl-pent-2-enoate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

10.8 g of p-toluenesulphonic acid×4 H2O are added to 500 g (3.16 mol) of ethyl isobutyrylacetate in 1,500 ml of toluene p.a., the mixture is saturated with ammonia gas while stirring at room temperature and allowed to stand overnight. It is then heated under reflux in a water separator and ammonia gas is continuously introduced until the calculated amount of water has separated (47 ml of water after reflux for 8 hours). The mixture is allowed to cool overnight, and the precipitate which has deposited is filtered off with suction and washed with toluene. The combined toluene phases are washed several times with water, dried using sodium sulphate, concentrated in vacuo and distilled in a high vacuum.

後処理

  1. temperatureIt is then heated
  2. customhas separated
  3. temperature(47 ml of water after reflux for 8 hours)
  4. temperatureto cool overnight
  5. filtrationthe precipitate which has deposited is filtered off with suction
  6. washwashed with toluene
  7. washThe combined toluene phases are washed several times with water
  8. customdried
  9. concentrationconcentrated in vacuo
  10. distillationdistilled in a high vacuum

出典と根拠

ORDレコード
ord-df9dac4e3ee44848a058c685983c1cf1
出典データセット
uspto-grants-1995_05
特許番号
US05418243

関連ノート

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