Hydrochloric Acid → Hydrochloric Acid

HRID 1277596ノート

反応式

HRID 1277596 の反応式
C([O:8][C:9]1[CH:29]=[CH:28][C:12]([O:13][CH2:14][CH2:15][N:16]2[CH2:21][CH2:20][N:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:18][CH2:17]2)=[CH:11][CH:10]=1)C1C=CC=CC=1.[ClH:30]>CCO>[OH:8][C:9]1[CH:10]=[CH:11][C:12]([O:13][CH2:14][CH2:15][N:16]2[CH2:17][CH2:18][N:19]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:20][CH2:21]2)=[CH:28][CH:29]=1.[ClH:30]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 129411031-[2-(4-Benzyloxyphenoxy)ethyl]-4-phenylpiperazine

生成物 2

HCID 313Hydrochloric AcidHCID 129411041-[2-(4-Hydroxyphenoxy)ethyl]-4-phenylpiperazine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

35.75 g of 1-[2-(4-benzyloxyphenoxy)ethyl]-4-phenylpiperazine was added rapidly with stirring to 75 ml concentrated HCl and the mixture was heated on a steam bath for 15 minutes. During this time starting material dissolved and then a white crystalline solid began to form and eventually the reaction mixture almost solidified. The reaction was cooled to ~5° and then was diluted with 100 ml EtOH. The solids were filtered off and were washed in EtOH and ether to give 1-[2-(4-hydroxyphenoxy)ethyl]-4-phenylpiperazine as its monohydrochloride. The salt was dissolved in 150 ml hot MeOH and 50 ml H2O and was then treated with 25 ml triethylamine. Water was then added to the refluxing mixture just to the cloud point whereupon the product began to crystallize from solution. The mixture was chilled and the solids were collected by filtration to give the end product, mp 142°-143°.

後処理

  1. temperaturethe mixture was heated on a steam bath for 15 minutes
  2. dissolutiondissolved
  3. customto form
  4. temperatureThe reaction was cooled to ~5°
  5. filtrationThe solids were filtered off
  6. washwere washed in EtOH

出典と根拠

ORDレコード
ord-72e2059f7a4c4038924b123fd4c35b59
出典データセット
uspto-grants-1981_07
特許番号
US04278608

反応ノート

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