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Isopropanol → 5,5-Dimethyl-1-(2-((4-(3-phenyl-2-thienyl)-2-pyrimidinyl)amino)ethyl)-2,4-imidazolidinedione

HRID 2267400
ノート
印刷プレビュー

反応式

HRID 2267400 の反応式
CN(C)[CH:3]=[CH:4][C:5]([C:7]1[S:8][CH:9]=[CH:10][C:11]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)=O.Cl.[CH3:20][C:21]1([CH3:34])[N:25]([CH2:26][CH2:27][NH:28][C:29]([NH2:31])=[NH:30])[C:24](=[O:32])[NH:23][C:22]1=[O:33].[OH-].[Na+].CC(O)C>ClCCl.O>[CH3:20][C:21]1([CH3:34])[N:25]([CH2:26][CH2:27][NH:28][C:29]2[N:31]=[C:5]([C:7]3[S:8][CH:9]=[CH:10][C:11]=3[C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:4]=[CH:3][N:30]=2)[C:24](=[O:32])[NH:23][C:22]1=[O:33]
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 3776IsopropanolHCID 14798Sodium HydroxideHCID 684650323-(Dimethylamino)-1-(3-phenylthiophen-2-yl)prop-2-en-1-oneHCID 1784294231-(2-(5,5-Dimethyl-2,4-dioxoimidazolidin-1-yl)ethyl)guanidine hydrochloride

生成物 1

HCID 602045225,5-Dimethyl-1-(2-((4-(3-phenyl-2-thienyl)-2-pyrimidinyl)amino)ethyl)-2,4-imidazolidinedione収率 33%

試薬・触媒・溶媒

2
HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

A flask charged with 3-(dimethylamino)-1-(3-phenylthiophen-2-yl)prop-2-en-1-one (52 mg, 0.20 mmol), 1-(2-(5,5-dimethyl-2,4-dioxoimidazolidin-1-yl)ethyl)guanidine hydrochloride (100 mg, 0.40 mmol) and sodium hydroxide (40 mg, 1.0 mmol) and IPA (3.0 mL) was heated to reflux under nitrogen. After 18 h, the reaction mixture was allowed to cool and then diluted with dichloromethane and water. The organic layer was separated and washed with one portion of water and two portions of brine. The organics were then concentrated and the residue purified by preparative TLC eluted with 3% MeOH/dichloromethane to afford the product (27 mg, 0.066 mmol, 33% yield). MS (M+H)+ 408.

後処理

  1. temperaturewas heated
  2. temperatureto reflux under nitrogen
  3. temperatureto cool
  4. customThe organic layer was separated
  5. washwashed with one portion of water and two portions of brine
  6. concentrationThe organics were then concentrated
  7. customthe residue purified by preparative TLC
  8. washeluted with 3% MeOH/dichloromethane

出典と根拠

ORDレコード
ord-9435be50b2b54763bf5effd79a3f5d96
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858785B2

反応ノート

読み込み中…

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