N,N-Diisopropylmethylamine → (R)-2-(4-Chloro-2-(2,4-dimethoxybenzyl)-7-fluoro-3-oxo-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-6-ylamino)-4-methylpentanamide

関与物質

役割	名称	HCID	仕込み量
反応物	N,N-Diisopropylmethylamine	HCID 547370	—
反応物	(R)-2-Amino-4-methylpentanamide	HCID 7271815	—
反応物	4,6-dichloro-2-[(2,4-dimethoxyphenyl)methyl]-7-fluoro-1H,2H,3H-pyrrolo[3,4-c]pyridin-3-one	HCID 58317575	—
溶媒	Acetonitrile	HCID 6342	—
溶媒	MeOH DCM DMF	HCID 86602994	—
生成物	(R)-2-(4-Chloro-2-(2,4-dimethoxybenzyl)-7-fluoro-3-oxo-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-6-ylamino)-4-methylpentanamide	HCID 58317560	33.1%

反応条件

温度	85 °C

反応手順

A mixture of 4,6-dichloro-2-(2,4-dimethoxybenzyl)-7-fluoro-1H-pyrrolo[3,4-c]pyridin-3(2H)-one (200 mg, 0.539 mmol), (R)-2-amino-4-methylpentanamide (140 mg, 1.078 mmol), and N-isopropyl-N-methylpropan-2-amine (310 mg, 2.69 mmol) in acetonitrile (2 mL) was stirred at 85° C. for 3 d. The resulting crude material was reconstituted in MeOH/DCM/DMF (10.0 mL) and purified via preparative HPLC. The fractions were collected and stripped to dryness via rotary evaporation to yield the title compound (83 mg, 33%). [M+H] calc'd for C22H26ClFN4O4, 465. found, 465.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US09181255B2
出典データセット	uspto-grants-2015_11
ORD ID	ord-0f611d64ff7f4ba19e623cf1293411c9
出典メモ	uspto-grants-2015_11