Ethyl orthoformate → HCID 135485944, 화합물

반응식

[NH2:1][C:2]1[N:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=[O:5].[CH:12](OCC)(OCC)OCC>>[F:11][C:9]1[CH:8]=[CH:7][C:3]2[C:4](=[O:5])[NH:6][CH:12]=[N:1][C:2]=2[N:10]=1

참가 물질

반응물 2

HCID 31214Ethyl orthoformate

HCID 131513852-Amino-6-fluoronicotinamide

생성물 1

HCID 135485944HCID 135485944, 화합물수율 96%

실험 절차

A suspension of 2-amino-6-fluoronicotinamide (0.74 g, 4.77 mmol) in triethyl orthoformate (25 mL) is heated at reflux for 8 h. After cooling to room temperature the precipitate is filtered off and washed well with petroleum ether to give 7-fluoropyrido[2,3-d]pyrimid-4(3H)-one (0.76 g, 96%). 1H NMR (DMSO) δ 12.75 (1H, brs), 8.66 (1H, dd, J=10.4, 8.4 Hz), 8.38 (1H, s), 7.33 (1H, dd, J=8.4, 2.6 Hz).

후처리

temperatureis heated
temperatureat reflux for 8 h
filtrationis filtered off
washwashed well with petroleum ether

출처 및 근거

ORD 기록: ord-5f94c60c0dcc4b41b09354dd940beb39
출처 데이터셋: uspto-grants-2000_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US06084095

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