Potassium Carbonate → 7-chloro-1,2-dimethyl-2,3-dihydroimidazo[1,2-c]pyrimidin-5(1H)-one

反応式

CS(O[CH2:6][CH:7]([N:9]([C:11]1[NH:12][C:13](=[O:18])[N:14]=[C:15]([Cl:17])[CH:16]=1)[CH3:10])[CH3:8])(=O)=O.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[Cl:17][C:15]1[CH:16]=[C:11]2[N:9]([CH3:10])[CH:7]([CH3:8])[CH2:6][N:12]2[C:13](=[O:18])[N:14]=1

参加物

反応条件

温度: 80 °C

実験手順

A mixture of 2-((6-chloro-2-oxo-2,3-dihydropyrimidin-4-yl)(methyl)amino)propyl methanesulfonate (800 mg, 2.71 mmol) and K2CO3 (748 mg, 5.41 mmol) in acetonitrile (6 mL) was stirred at 80° C. for 3 h, cooled to room temperature and concentrated. Purification via Biotage Spla HPFC system (C18, mobile phase: 0.01% NH4HCO3/H2O, 10˜95% CH3CN, 9.5 min, 30 mL/min) afforded the title product as an orange solid.

後処理

temperaturecooled to room temperature
concentrationconcentrated
customPurification via Biotage Spla HPFC system (C18, mobile phase: 0.01% NH4HCO3/H2O, 10˜95% CH3CN, 9.5 min, 30 mL/min)

出典と根拠

ORDレコード: ord-ed1ee36cd36646ecb8f6ff63b31b8b72
出典データセット: uspto-grants-2015_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09051325B2

反応ノート

読み込み中…

参加物

反応物 2

HCID 11430Potassium Carbonate

HCID 178460599HCID 178460599、化合物

生成物 1

HCID 867283147-chloro-1,2-dimethyl-2,3-dihydroimidazo[1,2-c]pyrimidin-5(1H)-one

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度: 80 °C

実験手順

後処理

temperaturecooled to room temperature
concentrationconcentrated
customPurification via Biotage Spla HPFC system (C18, mobile phase: 0.01% NH4HCO3/H2O, 10˜95% CH3CN, 9.5 min, 30 mL/min)

出典と根拠

ORDレコード: ord-ed1ee36cd36646ecb8f6ff63b31b8b72
出典データセット: uspto-grants-2015_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09051325B2

反応ノート

読み込み中…