Triethylamine → 4-Chloro-6-((2,6-difluorophenyl)amino)-2-(methylthio)pyrimidine-5-carbaldehyde

참여 물질

역할	이름	HCID	투입량
반응물	Triethylamine	HCID 8471	—
반응물	2,6-Difluoroaniline	HCID 79647	—
반응물	4,6-Dichloro-2-(methylsulfanyl)pyrimidine-5-carbaldehyde	HCID 4614004	—
용매	Tetrahydrofuran	HCID 8028	—
생성물	4-Chloro-6-((2,6-difluorophenyl)amino)-2-(methylthio)pyrimidine-5-carbaldehyde	HCID 9944737	70%

반응 조건

온도	55 °C

반응 단계

To a solution of 4,6-dichloro-2-(methylthio)-5-pyrimidinecarbaldehyde (10.0 g, 44.8 mmol) in THF (250 mL) was added 2,6-difluoroaniline (5.35 mL, 49.3 mmol, 1.1 eq) followed by Et3N (12.6 mL, 89.6 mmol, 2 eq). The reaction mixture was heated to 55° C. for about 22 h before concentrated. The slurry was re-dissolved in DCM (250 mL) and washed with H2O (2×100 mL), then concentrated and further washed with acetone (2×10 mL) to give 9.87 g (70%) of pure 4-chloro-6-[(2,6-difluorophenyl)amino]-2-(methylthio)-5-pyrimidinecarbaldehyde. LC-MS m/z 316 (M+H)+.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US08207176B2
출처 데이터셋	uspto-grants-2012_06
ORD ID	ord-bd6f464e9b9a48d2b4500249182b8351
출처 메모	uspto-grants-2012_06