반응 #487574

ord-2d090c3dd12842119556597e95e96285

반응 방정식

C1CCOC1
THF
O=Cc1c(Cl)nc(Cl)nc1Cl
2,4,6-tri-chloropyrimidine-5-carbaldehyde
CCOC(=O)CNN.Cl
ethyl hydrazinoacetate hydrochloride
CCOC(=O)Cn1ncc2c(Cl)nc(Cl)nc21
ethyl (4,6-dichloropyrazolo[3,4-d]pyrimidin-1-yl)acetate
수율 44.6%

반응 조건

온도
10°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The deposited precipitate is separated off (not the product)

실험 절차

155 ml of THF are added with stirring to a mixture of 5.17 g of 2,4,6-tri-chloropyrimidine-5-carbaldehyde and 5.85 g of ethyl hydrazinoacetate hydrochloride. The mixture is cooled to 10° C., and 6.78 ml of triethylamine are added dropwise. The mixture is stirred at RT for a further 1 h. The deposited precipitate is separated off (not the product). The filtrate, which contains the product, is subjected to conventional work-up, giving 3 g of ethyl (4,6-dichloropyrazolo[3,4-d]pyrimidin-1-yl)acetate (“12”).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08741896B2uspto-grants-2014_06