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HRID 324415作成日:2026年10月26日

Boron trifluoride etherate → (+/-)-5-(7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-2,4(1H,3H)-pyrimidinedione

https://huagongshe.com/reaction/324415

反応式

関与物質

役割名称HCID仕込み量
反応物Boron trifluoride etherateHCID 8000—
反応物TriethylsilaneHCID 12052—
反応物Sodium BicarbonateHCID 516892—
反応物(+/-)-4-(2,4-Bis(1,1-dimethylethoxy)pyrimidin-5-yl)-7-ethyl-2-methyl-9,10-dihydro-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-olHCID 70113732—
溶媒DichloromethaneHCID 6344—
生成物(+/-)-5-(7-Ethyl-9,10-dihydro-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-2,4(1H,3H)-pyrimidinedioneHCID 70114236—

反応条件

温度0 °C

反応手順

A stirred solution of the product from step (i) (0.60 g) in dichloromethane (15 ml) was treated with triethylsilane (0.225 ml) and cooled to 0° C. Boron trifluoride etherate (0.65 ml) was added in four equal portions at 5 minute intervals and the reaction stirred at room temperature for 16 hours. The reaction was poured into saturated sodium bicarbonate solution (200 ml) and extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated to give a yellow solid which was purified by reverse phase chromatography eluting with 50% to 80% methanol in 0.1% aqueous ammonium acetate.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06218376B1
出典データセットuspto-grants-2001_04
ORD IDord-81e57e3676454468b17fdd38b48e4ab2
出典メモuspto-grants-2001_04