1,4-Dioxane → HCID 178430894、化合物

反応式

CS([C:5]1[N:10]=[C:9]([C:11]2[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=2)[C:8]([CH3:17])=[CH:7][N:6]=1)(=O)=O.[O:18]1CCOCC1>>[CH3:17][C:8]1[C:9]([C:11]2[CH:12]=[N:13][CH:14]=[CH:15][CH:16]=2)=[N:10][C:5](=[O:18])[NH:6][CH:7]=1

参加物

反応物 2

HCID 312751,4-Dioxane

HCID 686973182-Methanesulfonyl-5-methyl-4-pyridin-3-yl-pyrimidine

生成物 1

HCID 178430894HCID 178430894、化合物収率 97%

実験手順

2-Methanesulfonyl-5-methyl-4-pyridin-3-yl-pyrimidine (1.3 g, 5.22 mmol) was dissolved in dioxane (80 ml) and then 2N NaOHaq (21 ml, 42 mmol) was added dropwise at room temperature. After stirring for 1 hour, the solution was neutralized with 37% HClaq. The residue was purified by flash chromatography with DCM-MeOH—NH4OH (9-1-0.1) to give 951 mg of the title compound as a light brown powder. (97% yield).

後処理

addition2N NaOHaq (21 ml, 42 mmol) was added dropwise at room temperature
customThe residue was purified by flash chromatography with DCM-MeOH—NH4OH (9-1-0.1)

出典と根拠

ORDレコード: ord-3c1658f842d34d9a858c62de445ea44c
出典データセット: uspto-grants-2012_07
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08222266B2

反応ノート

読み込み中…

参加物