Hydrochloric Acid → 2-(Phenethylhydrazono)-propionic acid

HRID 2163685ノート

反応式

HRID 2163685 の反応式
Cl[C:2](Cl)([CH3:6])[C:3]([OH:5])=[O:4].C(=O)([O-])[O-].[K+].[K+].Cl.[CH2:15]([NH:23][NH2:24])[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.Cl>O.CCOCC>[CH2:15]([NH:23][N:24]=[C:2]([CH3:6])[C:3]([OH:5])=[O:4])[CH2:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6418DalaponHCID 11430Potassium Carbonate3 回HCID 154983Phenelzine hydrochloride

生成物 1

HCID 1942362-(Phenethylhydrazono)-propionic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒3 回HCID 3283Diethyl Ether溶媒

反応条件

温度
90 °C

実験手順

To a solution of 5.7 g. 2,2-dichloropropionic acid and 2.8 g. potassium carbonate in 40 ml water is added a solution of 6.9 g. phenethylhydrazine hydrochloride and 5.6 g. potassium carbonate in 20 ml water. The mixture is heated with stirring to 90° C., a further solution of 5.6 g. potassium carbonate in 20 ml water is dropped in over 30 minutes and further stirred for 60 minutes at 90° C. Afterwards the still alkaline solution is cooled to ambient temperature, shaken out with ether and acidified with concentrated hydrochloric acid. 2-(phenethylhydrazono)-propionic acid crystallizes out and is recrystallized from toluene. The yield is 3.3 g. (40% of theory); m.p. 74°-76° C.

後処理

  1. temperatureThe mixture is heated
  2. stirringfurther stirred for 60 minutes at 90° C
  3. temperatureAfterwards the still alkaline solution is cooled to ambient temperature
  4. custom2-(phenethylhydrazono)-propionic acid crystallizes out
  5. customis recrystallized from toluene

出典と根拠

ORDレコード
ord-9ff0f9e9bbc2492a8ed7624fbdfde6a2
出典データセット
uspto-grants-1979_01
特許番号
US04136196

反応ノート

読み込み中…