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

Cesium carbonate → 4-(5-Bromothiophen-2-yl)-2-(2-(2-oxoimidazolidin-1-yl)ethylamino)pyrimidine-5-carbonitrile

HRID 507659
ノート
印刷プレビュー

反応式

HRID 507659 の反応式
[Br:1][C:2]1[S:3][C:4]([C:7]([C:9](=[CH:12]N(C)C)[C:10]#[N:11])=O)=[CH:5][CH:6]=1.Cl.[O:17]=[C:18]1[NH:22][CH2:21][CH2:20][N:19]1[CH2:23][CH2:24][NH:25][C:26]([NH2:28])=[NH:27].C(=O)([O-])[O-].[Cs+].[Cs+]>CN1CCCC1=O.CO>[Br:1][C:2]1[S:3][C:4]([C:7]2[C:9]([C:10]#[N:11])=[CH:12][N:28]=[C:26]([NH:25][CH2:24][CH2:23][N:19]3[CH2:20][CH2:21][NH:22][C:18]3=[O:17])[N:27]=2)=[CH:5][CH:6]=1
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

6

反応物 3

HCID 10796Cesium carbonateHCID 543239012-(2-Bromothiophene-5-carbonyl)-3-(dimethylamino)acrylonitrileHCID 178479475HCID 178479475、化合物

生成物 1

HCID 602045694-(5-Bromothiophen-2-yl)-2-(2-(2-oxoimidazolidin-1-yl)ethylamino)pyrimidine-5-carbonitrile

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 13387
N-methyl-2-pyrrolidone
溶媒

反応条件

温度
100 °C

実験手順

2-(2-Bromothiophene-5-carbonyl)-3-(dimethylamino)acrylonitrile) (3 g, 10 mmol) in N-methyl pyrrolidone (15 mL) was treated with 1-(2-(2-oxoimidazolidin-1-yl)ethyl)guanidine hydrochloride (1 M solution in N-methyl pyrrolidone, 15 mL, 15 mmol) and cesium carbonate (3.4 g, 10 mmol). The mixture was heated at 100° C. overnight. The reaction was then allowed to cool to room temperature and poured onto crushed ice. The resulting solid that formed was suspended in hot methanol to give a yellow solid (2.3 g). The filtrate was concentrated and purified by flash chromatography using a gradient of 3 to 10% methanol in dichloromethane to obtain an additional 0.9 g of the desired product. Total yield=3.2 g. MS (M+H)+ 394.

後処理

  1. temperatureto cool to room temperature
  2. additionpoured
  3. customonto crushed ice
  4. customThe resulting solid that formed

出典と根拠

ORDレコード
ord-e65159ef63aa4e36a69ecfbb2049a575
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07786132B2

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