1-benzyl-N-methylpiperidin-4-amine → U 99363

HRID 361812

反応式

HRID 361812 の反応式
[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][CH3:15])[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Br[C:17]1[C:22]([O:23][CH2:24][CH3:25])=[CH:21][CH:20]=[CH:19][N:18]=1>C(Cl)Cl>[CH2:1]([N:8]1[CH2:13][CH2:12][CH:11]([N:14]([CH3:15])[C:17]2[C:22]([O:23][CH2:24][CH3:25])=[CH:21][CH:20]=[CH:19][N:18]=2)[CH2:10][CH2:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 41361281-benzyl-N-methylpiperidin-4-amineHCID 106319262-BROMO-3-ETHOXYPYRIDINE

生成物 1

HCID 133107U 99363

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 1-benzyl-4-(methylamino)piperidine (EXAMPLE 9, 2.92 g) and 2-bromo-3-ethoxypyridine (EXAMPLE 69, 1.44 g) is stirred at 160°-165° in a sealed tube for 2 days, diluted with methylene chloride (50 ml), washed with water (10 ml) and saline (10 ml), dried over sodium sulfate, and concentrated under reduced pressure. The residue is chromatographed on silica gel (230-400 mesh, 300 g; eluting with a gradient of ethyl acetate/hexane (10/90-50/50)) to give the title compound, C,H,N: Anal. Calcd for C20H27N3O1 : C=73.81, H=8.36, N=12.91-found: C=73.59, H=8.37, N=12.83.

後処理

  1. washwashed with water (10 ml) and saline (10 ml)
  2. dry with materialdried over sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue is chromatographed on silica gel (230-400 mesh, 300 g
  5. washeluting with a gradient of ethyl acetate/hexane (10/90-50/50))

出典と根拠

ORDレコード
ord-f46c67e942b3493db6a54f5c40fb808f
出典データセット
uspto-grants-1999_02
特許番号
US05866589

関連ノート

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