Isonicotinoyl chloride hydrochloride → Hydrochloric Acid

関与物質

役割	名称	HCID	仕込み量
反応物	Isonicotinoyl chloride hydrochloride	HCID 12262826	—
反応物	N-((1S,2R,3S,4R)-4-{2-((R)-3-Amino-pyrrolidin-1-yl)-6-[2,2-bis-(4-hydroxy-phenyl)-ethylamino]-purin-9-yl}-2,3-dihydroxy-cyclopentyl)-propionamide	HCID 66630815	—
溶媒	Tetrahydrofuran	HCID 8028	—
溶媒	N-methyl-2-pyrrolidone	HCID 13387	—
生成物	Hydrochloric Acid	HCID 313	—
生成物	N-{(R)-1-[6-[2,2-Bis-(4-hydroxy-phenyl)-ethylamino]-9-((1R,2S,3R,4S)-2,3-dihydroxy-4-propionylamino-cyclopentyl)-9H-purin-2-yl]-pyrrolidin-3-yl}-isonicotinamide hydrochloride	HCID 66629861	—

反応手順

A mixture comprising N-((1S,2R,3S,4R)-4-{2-((R)-3-amino-pyrrolidin-1-yl)-6-[2,2-bis-(4-hydroxy-phenyl)-ethylamino]-purin-9-yl}-2,3-dihydroxy-cyclopentyl)-propionamide (Example 22 step 4) (20 mg, 33 μmol) in THF (0.5 ml) and NMP (0.5 ml) is treated with TEA (13 mg, 0.13 mmol) followed by isonicotinoyl chloride hydrochloride (16 mg, 83 μmol). After stirring at room temperature for 2 hours, the solvent is removed in vacuo and purification by C-18 reverse phase column chromatography eluting with acetonitrile:water:HCl (0.1%) (gradient of 0 to 100% acetonitrile) yields the title compound. (MH+ 708.4)

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US08258141B2
出典データセット	uspto-grants-2012_09
ORD ID	ord-adb39d173d3d473fb85e1a6db5973e04
出典メモ	uspto-grants-2012_09