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HRID 2171872作成日:2026年10月25日

Acetic Acid → HCID 178442411、化合物

https://huagongshe.com/reaction/2171872

反応式

関与物質

役割名称HCID仕込み量
反応物Acetic AcidHCID 176—
反応物HydroxyureaHCID 3657—
反応物Sodium HydroxideHCID 14798—
反応物methyl 2,3-dibromo-5-((5-fluoro-2-(5-fluoro-1H-pyrrolo[2,3-b]pyridin-3-yl)pyrimidin-4-yl)amino)-6,6-dimethylheptanoateHCID 86714756—
溶媒MethanolHCID 887—
溶媒WaterHCID 962—
生成物HCID 178442411HCID 178442411—

反応手順

To a solution of NaOH (0.015 g) dissolved in water (0.410 mL) was added hydroxyurea (0.008 g, 0.100 mmol). The resulting mixture was stirred for 30 minutes before the dropwise addition of methyl 2,3-dibromo-5-((5-fluoro-2-(5-fluoro-1H-pyrrolo[2,3-b]pyridin-3-yl)pyrimidin-4-yl)amino)-6,6-dimethylheptanoate, 85a, (0.064 g, 0.110 mmol) in MeOH (0.150 mL). The solution was stirred for 6 hours before the addition of AcOH (0.031 mL). The residue was purified by reverse phase preparative HPLC to afford the desired product: 1H NMR (300 MHz, MeOD) δ 8.57 (dd, J=9.7, 2.8 Hz, 1H), 8.16 (d, J=5.5 Hz, 2H), 8.00 (d, J=4.1 Hz, 1H), 5.68 (s, 1H), 3.03 (ddd, J=27.4, 15.4, 12.3 Hz, 2H), 1.10 (d, J=3.3 Hz, 11H); LCMS Gradient 10-90%, 0.1% formic acid, 5 minutes, C18/ACN, RT=2.15 minutes (M+H) 416.04.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09051319B2
出典データセットuspto-grants-2015_06
ORD IDord-8529576a69794fbbb74459923dc1bf04
出典メモuspto-grants-2015_06