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

HRID 232335

反応式

HRID 232335 の反応式
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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5c272afe37204cc6941c112a84e35e56
出典データセット
uspto-grants-1989_07
特許番号
US04851526

関連ノート

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