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HRID 15923作成日:2026年10月25日

Triphenylphosphine → 3-{5-[4-(4-Bromo-2-fluorophenylamino)-1,5-dimethyl-6-oxo-1,6-dihydro-pyridin-3-yl]-tetrazol-1-yl}-propionitrile

https://huagongshe.com/reaction/15923

反応式

関与物質

役割名称HCID仕込み量
反応物TriphenylphosphineHCID 11776—
反応物AzidotrimethylsilaneHCID 78378—
反応物Diisopropyl azodicarboxylateHCID 5363146—
反応物4-(4-Bromo-2-fluorophenylamino)-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid (2-cyano-ethyl)-amideHCID 66674377—
溶媒AcetonitrileHCID 6342—
溶媒Ethyl AcetateHCID 8857—
生成物3-{5-[4-(4-Bromo-2-fluorophenylamino)-1,5-dimethyl-6-oxo-1,6-dihydro-pyridin-3-yl]-tetrazol-1-yl}-propionitrileHCID 6667443461%

反応手順

PPh3 (83 mg, 0.32 mmol) was added to a stirred suspension of 4-(4-bromo-2-fluorophenylamino)-1,5-dimethyl-6-oxo-1,6-dihydropyridine-3-carboxylic acid (2-cyano-ethyl)-amide (51 mg, 0.12 mmol) in MeCN (1.5 mL). DIAD (0.065 mL, 0.31 mmol) and TMSN3 (0.045 mL, 0.32) were added dropwise. After 22 hours, the reaction mixture was diluted with ethyl acetate and washed with water. The aqueous layer was extracted with ethyl acetate. The combined organic extracts were dried (MgSO4) and concentrated under reduced pressure. Purification by flash column chromatography gave clean desired product (33 mg, 61%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07732616B2
出典データセットuspto-grants-2010_06
ORD IDord-0b8af127f4334c3294b8f6645ddf672d
出典メモuspto-grants-2010_06