Hydrochloric Acid → Hydrochloric Acid

HRID 1155412노트

반응식

HRID 1155412 반응식
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]

참가 물질

5

반응물 2

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

생성물 2

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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 mixtue 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]-4phenylpiperazine 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°.

후처리

  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

출처 및 근거

ORD 기록
ord-35dc835596cb426793f3a85bda619497
출처 데이터셋
uspto-grants-1981_11
특허 번호
US04301300

반응 노트

불러오는 중…