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

Potassium Iodide → 1-Benzyl-2,6-diethyl-2,3,6-trimethyl-4-benzamidopiperidine

HRID 1701107
ノート
印刷プレビュー

反応式

HRID 1701107 の反応式
[CH2:1]([C:3]1([CH3:22])[CH:8]([CH3:9])[CH:7]([NH:10][C:11](=[O:18])[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:6][C:5]([CH2:20][CH3:21])([CH3:19])[NH:4]1)[CH3:2].[CH2:23](Br)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>S1(=O)(=O)CCCC1.C1(C)C=CC=CC=1>[CH2:23]([N:4]1[C:5]([CH2:20][CH3:21])([CH3:19])[CH2:6][CH:7]([NH:10][C:11](=[O:18])[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:8]([CH3:9])[C:3]1([CH2:1][CH3:2])[CH3:22])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 22486017N-(2,6-Diethyl-2,3,6-trimethylpiperidin-4-yl)benzamide

生成物 1

HCID 203483301-Benzyl-2,6-diethyl-2,3,6-trimethyl-4-benzamidopiperidine

試薬・触媒・溶媒 2

HCID 1140Toluene
溶媒
HCID 31347Sulfolane溶媒

実験手順

20 g of 2,6-diethyl-2,3,6-trimethyl-4-benzamidopiperidine (compound no. 9), 12.5 g of benzylbromide, 1 g of potassium iodide and 20 g of potassium carbonate are stirred in 200 ml of tetrahydrothiophene dioxide (sulpholane) at 110° C. for 4 days. Thereafter the reaction mixture is diluted with 200 ml of toluene, cooled to room temperature and purified by filtration. The filtrate is washed four times with about 200 ml of water, the toluene phase is dried over sodium sulfate and evaporated under vacuum. Crystallization of the residue from acetic acid ethyl ester yields 1-benzyl-2,6-diethyl-2,3,6-trimethyl-4-benzamidopiperidine (compound no. 48); m.p. 234°-236° C.

後処理

  1. filtrationpurified by filtration
  2. washThe filtrate is washed four times with about 200 ml of water
  3. dry with materialthe toluene phase is dried over sodium sulfate
  4. customevaporated under vacuum
  5. customCrystallization of the residue from acetic acid ethyl ester

出典と根拠

ORDレコード
ord-b3576292e75e412ab03c0bf3c6f01fdc
出典データセット
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04191683

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