ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Triethylamine → 1-[1(RS)-[1-(3,4-dichlorobenzyl)piperidin-4-ylmethyl]-2-methylpropyl}-4-methylbenzamide

HRID 1610911
ノート
印刷プレビュー

反応式

HRID 1610911 の反応式
[C:1]1([CH3:10])[CH:6]=[CH:5][C:4]([C:7](Cl)=[O:8])=[CH:3][CH:2]=1.[Cl:11][C:12]1[CH:13]=[C:14]([CH:28]=[CH:29][C:30]=1[Cl:31])[CH2:15][N:16]1[CH2:21][CH2:20][CH:19]([CH2:22][CH:23](N)[CH:24]([CH3:26])[CH3:25])[CH2:18][CH2:17]1.C([N:34](CC)CC)C>ClCCl>[Cl:11][C:12]1[CH:13]=[C:14]([CH:28]=[CH:29][C:30]=1[Cl:31])[CH2:15][N:16]1[CH2:21][CH2:20][CH:19]([CH2:22][CH:23]([C:4]2([CH:5]=[CH:6][C:1]([CH3:10])=[CH:2][CH2:3]2)[C:7]([NH2:34])=[O:8])[CH:24]([CH3:26])[CH3:25])[CH2:18][CH2:17]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 134054-Methylbenzoyl ChlorideHCID 222576661(RS)-[1-(3,4-dichlorobenzyl)piperidin-4-ylmethyl]-2-methylpropylamine

生成物 1

HCID 865889811-[1(RS)-[1-(3,4-dichlorobenzyl)piperidin-4-ylmethyl]-2-methylpropyl}-4-methylbenzamide収率 95.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

p-Toluoyl chloride (0.077 ml, 0.58 mmol) was added to a solution of 1(RS)-[1-(3,4-dichlorobenzyl)piperidin-4-ylmethyl]-2-methylpropylamine (0.16 g, 0.49 mmol) in dichloromethane (2 ml) and triethylamine (0.12 ml, 1.63 mmol). The reaction mixture was stirred at room temperature for 1.5 h and was quenched with water. The product was then extracted with dichloromethane and the organic layer was washed with brine and dried over sodium sulfate. The crude product was purified on preparative TLC with 25% acetone, 25% dichloromethane in hexanes to give 0.21 g of N-{1-[1(RS)-[1-(3,4-dichlorobenzyl)piperidin-4-ylmethyl]-2-methylpropyl}-4-methylbenzamide as an oil, which was then converted to its dihydrochloride salt (0.15 g); m.p. 233.9-235.5° C.

後処理

  1. customwas quenched with water
  2. extractionThe product was then extracted with dichloromethane
  3. washthe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. customThe crude product was purified on preparative TLC with 25% acetone, 25% dichloromethane in hexanes

出典と根拠

ORDレコード
ord-16f23ad938c146aaa2420ddc3dd3193b
出典データセット
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06984637B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート