Methanamine, N-methoxy-, hydrochloride (1:1) → 2-(N-Boc)amino-3-(4-cyanophenyl)-N-methoxy-N-methylpropanamide

関与物質

役割	名称	HCID	仕込み量
反応物	Methanamine, N-methoxy-, hydrochloride (1:1)	HCID 81138	—
反応物	Diisopropylethylamine	HCID 81531	—
反応物	O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate	HCID 2733207	—
反応物	N-(tert-Butoxycarbonyl)-4-cyano-L-phenylalanine	HCID 7020841	—
溶媒	Dichloromethane	HCID 6344	—
生成物	2-(N-Boc)amino-3-(4-cyanophenyl)-N-methoxy-N-methylpropanamide	HCID 21070238	—

反応手順

2 g of (N-Boc)-4-cyanophenylalanine, 2.32 g of TBTU, 2.40 ml of DIPEA and 806 mg of N,O-dimethylhydroxylamine hydrochloride are mixed together in 30 ml of DCM. After stirring for 24 hours at RT, the reaction mixture is concentrated to dryness and the residue is then extracted with EtOAc. The organic phase is washed with a pH 2 buffer solution, a saturated NaHCO3 solution and then a saturated NaCl solution. The expected compound crystallizes from a mixture of isopropyl ether and pentane (1.89 g).

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US07157454B2
出典データセット	uspto-grants-2007_01
ORD ID	ord-90a6d7c751cc4148b1a4a3cdbb4e6014
出典メモ	uspto-grants-2007_01