Dimethylformamide → HCID 22024352、化合物

反応式

[Br:1][C:2]1[C:3]2[N:4]([CH:8]=[C:9]([CH2:11][CH3:12])[N:10]=2)[CH:5]=[N:6][CH:7]=1.P(Cl)(Cl)(Cl)=O.CN(C)[CH:20]=[O:21]>>[Br:1][C:2]1[C:3]2[N:4]([C:8]([CH:20]=[O:21])=[C:9]([CH2:11][CH3:12])[N:10]=2)[CH:5]=[N:6][CH:7]=1

参加物

反応物 3

HCID 6228Dimethylformamide

HCID 24813Phosphorus oxychloride

HCID 22024358HCID 22024358、化合物

生成物 1

HCID 22024352HCID 22024352、化合物

実験手順

8-Bromo-2-ethylimidazo[1,2-c]pyrimidine (1.0 g) was added to a mixture of phosphorus oxychloride (1.2 mL) and N,N-dimethylformamide (4.4 mL) at room temperature. The mixture was heated under stirring as it was at 80° C. for 1 day. After cooled to room temperature, it was poured slowly on ice. The material was extracted with ethyl acetate and washed with water, and the solvent was evaporated. The resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:5) to give the title compound (0.5 g) as white crystals.

後処理

temperatureThe mixture was heated
additionit was poured slowly on ice
extractionThe material was extracted with ethyl acetate
washwashed with water
customthe solvent was evaporated
customThe resulting residue was purified by silica gel column chromatography (ethyl acetate:n-hexane=1:5)

出典と根拠

ORDレコード: ord-3cca3e00bbc64b42a99f319374361cd1
出典データセット: uspto-grants-2006_07
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US07078405B2

反応ノート

読み込み中…

参加物