Allyl bromide → 1-(4-Allyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanol

HRID 370664노트

반응식

HRID 370664 반응식
[C:1]1([CH:7]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH:15]([C:17]3[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=3)[OH:16])[CH2:10][CH2:9]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:30](Br)[CH:31]=[CH2:32].[OH-].[K+]>C(O)C>[CH2:32]([O:23][C:20]1[CH:19]=[CH:18][C:17]([CH:15]([OH:16])[CH2:14][N:11]2[CH2:10][CH2:9][N:8]([CH:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH2:13][CH2:12]2)=[CH:22][CH:21]=1)[CH:31]=[CH2:30]

참가 물질

5

반응물 3

HCID 7841Allyl bromideHCID 14797Potassium HydroxideHCID 30711602-(4-Diphenylmethylpiperazinyl)-1-(4-hydroxyphenyl)ethanol

생성물 1

HCID 103203901-(4-Allyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanol수율 64%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

In 1.2 liters of ethanol were dissolved 120 g (0.31 mol) of 2-(4-diphenylmethylpiperazinyl)-1-(4-hydroxyphenyl)-ethanol, 74.8 g (0.62 mol) of allyl bromide and 41 g of potassium hydroxide. The resultant solution was heated with refluxing for one hour. After cooling the solution and then removing the solvent, the residue was added with 1.0 liter of ethyl acetate. The resultant mixture was washed successively with an aqueous 1N solution of sodium hydroxide, water and saturated saline, followed by drying over anhydrous sodium sulfate. The solvent was removed, and the residue was crystallized from a mixed solvent of ethanol and n-hexane to give 84.6 g of 1-(4-allyloxyphenyl)-2-(4-diphenylmethylpiperazinyl)ethanol (yield: 64%).

후처리

  1. temperaturewith refluxing for one hour
  2. temperatureAfter cooling the solution
  3. customremoving the solvent
  4. additionthe residue was added with 1.0 liter of ethyl acetate
  5. washThe resultant mixture was washed successively with an aqueous 1N solution of sodium hydroxide, water and saturated saline
  6. dry with materialby drying over anhydrous sodium sulfate
  7. customThe solvent was removed
  8. customthe residue was crystallized from a mixed solvent of ethanol and n-hexane

출처 및 근거

ORD 기록
ord-0aac2fb3855742bda7200f6e4e9e1e46
출처 데이터셋
uspto-grants-1985_07
특허 번호
US04528194

반응 노트

불러오는 중…