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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 324427생성일: 2026년 10월 25일

5-Bromo-2,4-bis(1,1-dimethylethoxy)pyrimidine → (+/-)-5-(9,10-Dihydro-4-hydroxy-2,7-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-2,4(1H,3H)-pyrimidinedione

https://huagongshe.com/reaction/324427

반응식

참여 물질

역할이름HCID투입량
반응물5-Bromo-2,4-bis(1,1-dimethylethoxy)pyrimidineHCID 818851—
반응물9,10-Dihydro-2,7-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-oneHCID 22003633—
반응물ButyllithiumHCID 178418339—
용매Acetic AcidHCID 176—
용매TetrahydrofuranHCID 8028—
생성물(+/-)-5-(9,10-Dihydro-4-hydroxy-2,7-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-2,4(1H,3H)-pyrimidinedioneHCID 70113848—

반응 단계

To a solution of the product from example 1 step (vi) (9 g) in dry tetrahydrafuran (100 ml) under nitrogen at −78° C. was added n-butyllithium (2.5M, 14.3 ml) dropwise over 1 min. After 30 min a warm solution of the product from step (v) (6.73 g) in tetrahydrofuran (350 ml) was added rapidly via cannula. After further stirring for 1 h the cooling bath was removed and the mixture allowed to stir at room temperature for 30 min. The reaction mixture was quenched with saturated brine and extracted with ethyl acetate (×2). The combined organic extracts were dried over magnesium sulphate and solvent removed under reduced pressure to leave a pale yellow foam. This was dissolved in acetic acid (100 ml) and stired at room temperature for 16 h. The solvent was evaporated under reduced pressure and the residue azeotroped with toluene (×2) to remove last traces of acetic acid. The remaining residue was triturated with diethyl ether/isohexane mixtures and filtered to give the subtitle product as a beige solid.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US06218376B1
출처 데이터셋uspto-grants-2001_04
ORD IDord-65e682c4b4124404abedce50eb29b36c
출처 메모uspto-grants-2001_04