홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Potassium Iodide → 4'-Tert-butyl-4-[4-[alpha-hydroxy-alpha-(p-tolyl)benzyl]-piperidino]butyrophenone hydrochloride

HRID 1579326
노트
인쇄 미리보기

반응식

HRID 1579326 반응식
[C:1]1([C:7]([C:15]2[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=2)([CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[OH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:22]([C:26]1[CH:31]=[CH:30][C:29]([C:32](=[O:37])[CH2:33][CH2:34][CH2:35][Cl:36])=[CH:28][CH:27]=1)([CH3:25])([CH3:24])[CH3:23].C(=O)(O)[O-].[K+].[I-].[K+]>C1(C)C=CC=CC=1.O>[ClH:36].[C:22]([C:26]1[CH:27]=[CH:28][C:29]([C:32](=[O:37])[CH2:33][CH2:34][CH2:35][N:12]2[CH2:13][CH2:14][CH:9]([C:7]([OH:8])([C:15]3[CH:20]=[CH:19][C:18]([CH3:21])=[CH:17][CH:16]=3)[C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:10][CH2:11]2)=[CH:30][CH:31]=1)([CH3:25])([CH3:24])[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 516893Potassium BicarbonateHCID 27236944'-tert-Butyl-4-chlorobutyrophenoneHCID 21568361alpha-Phenyl-alpha-(p-tolyl)-4-piperidinemethanol

생성물 1

HCID 215683424'-Tert-butyl-4-[4-[alpha-hydroxy-alpha-(p-tolyl)benzyl]-piperidino]butyrophenone hydrochloride

시약·촉매·용매 2

HCID 962
Water
용매
HCID 1140Toluene용매2회

실험 절차

A mixture of 29.0 g (0.1 mole) of α-phenyl-α-(p-tolyl)-4-piperidinemethanol, 32 g (0.12 mole) of 4'-tert-butyl-4-chlorobutyrophenone, 20 g of potassium bicarbonate, 0.1 g of potassium iodide, 300 ml of toluene and 50 ml of water is stirred on a steam bath for 88 hours. Upon cooling to room temperature the toluene layer is separated, and the aqueous layer is extracted with toluene. The combined toluene fractions are washed with water and saturated sodium chloride solution, dried over magnesium sulfate, filtered and concentrated to an oil. The oily residue is dissolved in dry ether and filtered. The filtrate is treated with ethereal HCl, and the resulting precipitate is collected and recrystallized from methanol-butanone to give 4'-tert-butyl-4-[4-[α-hydroxy-α-(p-tolyl)benzyl]-piperidino]butyrophenone hydrochloride, M.P. 194°-196.5°C.

후처리

  1. customis separated
  2. extractionthe aqueous layer is extracted with toluene
  3. washThe combined toluene fractions are washed with water and saturated sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated to an oil
  7. dissolutionThe oily residue is dissolved in dry ether
  8. filtrationfiltered
  9. additionThe filtrate is treated with ethereal HCl
  10. customthe resulting precipitate is collected
  11. customrecrystallized from methanol-butanone

출처 및 근거

ORD 기록
ord-70a8fd652fee4eeda76ee9724cbc3fc0
출처 데이터셋
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03931197

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트