Ethyl chloroformate → Ethyl 4-(4-hydroxyphenyl)piperazine-1-carboxylate

HRID 614432ノート

反応式

HRID 614432 の反応式
Br.Br.[N:3]1([C:9]2[CH:14]=[CH:13][C:12]([OH:15])=[CH:11][CH:10]=2)[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1.[C:16](Cl)(=[O:20])[O:17][CH2:18][CH3:19].C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1>[OH:15][C:12]1[CH:11]=[CH:10][C:9]([N:3]2[CH2:4][CH2:5][N:6]([C:16]([O:17][CH2:18][CH3:19])=[O:20])[CH2:7][CH2:8]2)=[CH:14][CH:13]=1

参加物

5

反応物 3

HCID 10928Ethyl chloroformateHCID 11430Potassium CarbonateHCID 2723591p-(1-Piperazinyl)phenol dihydrobromide

生成物 1

HCID 2430972Ethyl 4-(4-hydroxyphenyl)piperazine-1-carboxylate

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 17 parts of 4-(1-piperazinyl)phenol dihydrobromide, 7 parts of ethyl carbonochloridate, 21 parts of potassium carbonate and 250 parts of 1,4-dioxane is stirred and refluxed for 48 hours. The reaction mixture is filtered, while hot and the filtrate is evaporated. The solid residue is dissolved in a diluted hydrochloric acid solution. The solution is alkalized with ammonium hydroxide. The product is filtered off and dried, yielding 3.5 parts of ethyl 4-(4-hydroxyphenyl)-1-piperazinecarboxylate; mp. 168.8° C.

後処理

  1. temperaturerefluxed for 48 hours
  2. filtrationThe reaction mixture is filtered
  3. customwhile hot and the filtrate is evaporated
  4. dissolutionThe solid residue is dissolved in a diluted hydrochloric acid solution
  5. filtrationThe product is filtered off
  6. customdried

出典と根拠

ORDレコード
ord-214bb38816fa4c549ac63523847a4fff
出典データセット
uspto-grants-1979_03
特許番号
US04144346

反応ノート

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