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

Dimethylhydantoin → 3-[4-(4-Pyridylthio)butyl]-5,5-dimethylhydantoin

HRID 6167
ノート
印刷プレビュー

反応式

HRID 6167 の反応式
[CH3:1][C:2]1([CH3:9])[NH:6][C:5](=[O:7])[NH:4][C:3]1=[O:8].Cl[CH2:11][CH2:12][CH2:13][CH2:14][S:15][C:16]1[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=1.C1CCN2C(=NCCC2)CC1.C(OCC)(=O)C>CN(C)C=O>[CH3:1][C:2]1([CH3:9])[NH:6][C:5](=[O:7])[N:4]([CH2:11][CH2:12][CH2:13][CH2:14][S:15][C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)[C:3]1=[O:8]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6491DimethylhydantoinHCID 8857Ethyl AcetateHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 158169784-(4-Chlorobutylthio)pyridine

生成物 1

HCID 190790983-[4-(4-Pyridylthio)butyl]-5,5-dimethylhydantoin収率 56.8%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To a solution of 2.56 g (20 mmol) of 5,5-dimethylhydantoin and 4.03 g (20 mmol) of 4-(4-chlorobutylthio)pyridine in 20 ml of N,N-dimethylformamide, 3.00 ml (20 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene was added, and the mixture was stirred at room temperature for 43 hours, followed by further stirring at 70° C. for 10 hours. Ethyl acetate was added to the reaction mixture, and the mixture was washed three times with water and dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by column chromatography (eluent: ethyl acetate/ethanol =10:1) to give 3.33 g of the desired compound (56.8% yield, colorless crystals).

後処理

  1. stirringby further stirring at 70° C. for 10 hours
  2. washthe mixture was washed three times with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off
  5. customthe residue was purified by column chromatography (eluent: ethyl acetate/ethanol =10:1)

出典と根拠

ORDレコード
ord-223b53ba401c4783b307cafc7579f4f4
出典データセット
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05246948

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