Tetrahydrofuran → 4-(1H-Imidazol-1-yl)phenyl-4-methyl-1-piperidine ethanol

HRID 232335

반응식

HRID 232335 반응식
Br[CH2:2][CH:3]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH:15]=[CH:14][N:13]=[CH:12]2)=[CH:7][CH:6]=1)O.[CH3:16][CH:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.[O:23]1CCCC1>>[N:11]1([C:8]2[CH:9]=[CH:10][C:5]([CH:3]3[CH2:2][CH:17]([CH3:16])[CH2:18][CH2:19][N:20]3[CH2:21][CH2:22][OH:23])=[CH:6][CH:7]=2)[CH:15]=[CH:14][N:13]=[CH:12]1

참가 물질

4

반응물 3

HCID 8028TetrahydrofuranHCID 693814-MethylpiperidineHCID 20031362alpha-(Bromomethyl)-4-(1H-imidazol-1-yl)benzenemethanol

생성물 1

HCID 178455204-(1H-Imidazol-1-yl)phenyl-4-methyl-1-piperidine ethanol

실험 절차

Add α-(bromomethyl)-4-(1H-imidazol-1-yl)benzenemethanol (8.88 g, 33.24 mmol) to a room temperature solution of 4-methylpiperidine (11.8 mL, 99.73 mmol) in tetrahydrofuran (90mL). Stir the resultant mixture for 2.5 days and concentrate in vacuo. Chromatograph the residue on alumina (neutral, activity III, 100 g) using first methylene chloride than 2% methanol in methylene chloride as eluent. Collect the product fraction and concentrate in vacuo to give a solid. Recrystallize the solid from petroleum ether/ethyl acetate (ca. 4+1). Drying at 50° C. for 2 hr at p=1.0 mm affords the title compound.

후처리

  1. concentrationconcentrate in vacuo
  2. customCollect the product fraction
  3. concentrationconcentrate in vacuo
  4. customto give a solid
  5. customRecrystallize the solid from petroleum ether/ethyl acetate (ca. 4+1)
  6. customDrying at 50° C. for 2 hr at p=1.0 mm

출처 및 근거

ORD 기록
ord-5c272afe37204cc6941c112a84e35e56
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04851526

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