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

Pyridinium chloride → N-(4-(Dimethylphosphoryl)phenyl)-9-vinyl-9H-purin-6-amine

HRID 655794
ノート
印刷プレビュー

反応式

HRID 655794 の反応式
Cl[C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[CH:11]=[CH2:12].[CH3:13][P:14]([CH3:23])([C:16]1[CH:22]=[CH:21][C:19]([NH2:20])=[CH:18][CH:17]=1)=[O:15].Cl.N1C=CC=CC=1>C(OCCO)C>[CH3:23][P:14]([C:16]1[CH:22]=[CH:21][C:19]([NH:20][C:2]2[N:10]=[CH:9][N:8]=[C:7]3[C:3]=2[N:4]=[CH:5][N:6]3[CH:11]=[CH2:12])=[CH:18][CH:17]=1)([CH3:13])=[O:15]
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

5

反応物 3

HCID 10176127Pyridinium chlorideHCID 109541366-Chloro-9-vinyl-9H-purineHCID 206345534-(Dimethylphosphoryl)aniline

生成物 1

HCID 68925961N-(4-(Dimethylphosphoryl)phenyl)-9-vinyl-9H-purin-6-amine

試薬・触媒・溶媒 1

HCID 8076Glycol monoethyl ether溶媒

反応条件

温度
160 °C

実験手順

A mixture of 6-chloro-9-vinylpurine (0.18 g, 1 mmol), 4-dimethylphosphinylaniline (0.17 g, 1 mmol), and pyridine hydrochloride (0.11 g, 1 mmol) was dissolved in 2-ethoxyethanol (2 mL). The resulting solution was heated at 160° C. for 10 minutes under microwave irradiation. The mixture was concentrated to dryness on a rotavap. EtOAc and aq. NaHCO3 were added. The aqueous layer was extracted with ethyl acetate and the combined organic layers were dried over sodium sulfate, concentrated on a rotavap, and then subjected to silica gel column chromatography (eluent: 10% methanol/methylene chloride) yielding the desired product.

後処理

  1. concentrationThe mixture was concentrated to dryness on a rotavap
  2. additionEtOAc and aq. NaHCO3 were added
  3. extractionThe aqueous layer was extracted with ethyl acetate
  4. dry with materialthe combined organic layers were dried over sodium sulfate
  5. concentrationconcentrated on a rotavap

出典と根拠

ORDレコード
ord-02834ddfa82945d3bcfe0397c4dbb1f0
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08071609B2

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