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

Hydrogen Peroxide → 2-[(3-hydroxypropyl)amino]-4-{4-[6-(trifluoromethyl)pyridin-3-yl]-9H-carbazol-9-yl}benzamide

HRID 1877482
ノート
印刷プレビュー

反応式

HRID 1877482 の反応式
C(=O)([O-])[O-:2].[K+].[K+].[NH2:7][CH2:8][CH2:9][CH2:10][OH:11].F[C:13]1[CH:20]=[C:19]([N:21]2[C:33]3[CH:32]=[CH:31][CH:30]=[C:29]([C:34]4[CH:35]=[N:36][C:37]([C:40]([F:43])([F:42])[F:41])=[CH:38][CH:39]=4)[C:28]=3[C:27]3[C:22]2=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH:18]=[CH:17][C:14]=1[C:15]#[N:16].[OH-].[Na+].OO>CS(C)=O.O.C(O)C>[OH:11][CH2:10][CH2:9][CH2:8][NH:7][C:13]1[CH:20]=[C:19]([N:21]2[C:33]3[CH:32]=[CH:31][CH:30]=[C:29]([C:34]4[CH:35]=[N:36][C:37]([C:40]([F:43])([F:42])[F:41])=[CH:38][CH:39]=4)[C:28]=3[C:27]3[C:22]2=[CH:23][CH:24]=[CH:25][CH:26]=3)[CH:18]=[CH:17][C:14]=1[C:15]([NH2:16])=[O: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

9

反応物 5

HCID 784Hydrogen PeroxideHCID 90863-Amino-1-propanolHCID 11430Potassium CarbonateHCID 14798Sodium HydroxideHCID 673087102-fluoro-4-{4-[6-(trifluoromethyl)pyridin-3-yl]-9H-carbazol-9-yl}benzonitrile

生成物 1

HCID 583383562-[(3-hydroxypropyl)amino]-4-{4-[6-(trifluoromethyl)pyridin-3-yl]-9H-carbazol-9-yl}benzamide

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

0.17 g of potassium carbonate and 0.64 ml of 3-amino-1-propanol are successively added to a solution of 0.18 g of 2-fluoro-4-{4-[6-(trifluoromethyl)pyridin-3-yl]-9H-carbazol-9-yl}benzonitrile in 2 ml of dimethyl sulphoxide. The reaction mixture is heated at 90° C. for 1 hour 20 minutes in a microwave, and then 4.2 ml of ethanol are added, followed by 0.8 ml of a 1N solution of sodium hydroxide and 0.8 ml of 30% aqueous hydrogen peroxide. The reaction mixture is stirred at ambient temperature for 2 hours and then diluted with distilled water. The aqueous phase is extracted twice with ethyl acetate and the combined organic phases are washed with water and a saturated solution of sodium chloride, dried over magnesium sulphate and concentrated under reduced pressure. The white solid obtained is purified by silica gel chromatography, elution being carried out with a mixture of dichloromethane, acetonitrile and methanol (96/2/2 by volume) so as to give 24 mg of 2-[(3-hydroxypropyl)amino]-4-{4-[6-(trifluoromethyl)pyridin-3-yl]-9H-carbazol-9-yl}benzamide in the form of a white solid, the characteristics of which are the following

後処理

  1. extractionThe aqueous phase is extracted twice with ethyl acetate
  2. washthe combined organic phases are washed with water
  3. dry with materiala saturated solution of sodium chloride, dried over magnesium sulphate
  4. concentrationconcentrated under reduced pressure
  5. customThe white solid obtained
  6. customis purified by silica gel chromatography, elution
  7. additionbeing carried out with a mixture of dichloromethane, acetonitrile and methanol (96/2/2 by volume) so as

出典と根拠

ORDレコード
ord-f90fb428c9194e929b6d6ee9c3aa5867
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08309721B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート