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Methyl iodide → (R)-1-[2-(4-Pyridyl)ethyl]-2-pyrrolidinecarboxylic acid N-[2-(1-adamantyl)ethyl]-1-pentylamide hydrochloride

HRID 11482
ノート
印刷プレビュー

反応式

HRID 11482 の反応式
Cl.[C:2]12([CH2:12][CH2:13][N:14]([CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[C:15]([C@H:17]3[CH2:21][CH2:20][CH2:19][NH:18]3)=[O:16])[CH2:11][CH:6]3[CH2:7][CH:8]([CH2:10][CH:4]([CH2:5]3)[CH2:3]1)[CH2:9]2.C(=O)([O-])[O-].[K+].[K+].CI.Cl.[Cl:36][CH2:37][CH2:38][C:39]1[CH:44]=[CH:43][N:42]=[CH:41][CH:40]=1.[OH-].[Na+]>CN(C)C=O.C(OCC)C>[ClH:36].[C:2]12([CH2:12][CH2:13][N:14]([CH2:22][CH2:23][CH2:24][CH2:25][CH3:26])[C:15]([C@H:17]3[CH2:21][CH2:20][CH2:19][N:18]3[CH2:37][CH2:38][C:39]3[CH:44]=[CH:43][N:42]=[CH:41][CH:40]=3)=[O:16])[CH2:9][CH:8]3[CH2:10][CH:4]([CH2:5][CH:6]([CH2:7]3)[CH2:11]1)[CH2:3]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 124817414-(2-Chloroethyl)pyridine hydrochlorideHCID 67118563HCID 67118563、化合物

生成物 1

HCID 67118947(R)-1-[2-(4-Pyridyl)ethyl]-2-pyrrolidinecarboxylic acid N-[2-(1-adamantyl)ethyl]-1-pentylamide hydrochloride
収率 47%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

Next, (R)-2-pyrrolidinecarboxylic acid N-[2-(1-adamantyl)ethyl]-N-pentylamide hydrochloride (1.4 g, 3.7 mmol) was dissolved in anhydrous N,N-dimethylformamide (40 ml), potassium carbonate (2.6 g, 19 mmol), methyl iodide (1.7 g, 11 mmol) and 4-(2-chloroethyl)pyridine hydrochloride (0.70 g, 3.7 mmol) were added to the solution, and the mixture was stirred at an external temperature of 80° C. overnight. A 2 N aqueous sodium hydroxide solution (70 ml) and diethyl ether (70 ml) were added to the reaction mixture, the reaction mixture was distributed, and the diethyl ether layer was washed with water (70 ml) and a saturated aqueous sodium chloride solution (70 ml) successively and dried over anhydrous magnesium sulfate. The diethyl ether layer was concentrated under reduced pressure, and the concentrate was purified by silica gel column chromatography to give 0.80 g (47%) of the titled compound as an oily matter.

後処理

  1. washthe diethyl ether layer was washed with water (70 ml)
  2. dry with materiala saturated aqueous sodium chloride solution (70 ml) successively and dried over anhydrous magnesium sulfate
  3. concentrationThe diethyl ether layer was concentrated under reduced pressure
  4. customthe concentrate was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-69caa58474a641298e579f0a71042a19
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07098226B2

反応ノート

読み込み中…

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