Dimethylformamide → HCID 22024352, 화합물

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[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

참가 물질

반응물 3

HCID 6228Dimethylformamide

HCID 24813Phosphorus oxychloride

HCID 22024358HCID 22024358, 화합물

생성물 1

HCID 22024352HCID 22024352, 화합물

실험 절차

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.

후처리

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)

출처 및 근거

ORD 기록: ord-3cca3e00bbc64b42a99f319374361cd1
출처 데이터셋: uspto-grants-2006_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07078405B2

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