Diisopropylethylamine → HCID 123681539、化合物

関与物質

役割	名称	HCID	仕込み量
反応物	Diisopropylethylamine	HCID 81531	—
反応物	O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate	HCID 2733207	—
反応物	(3-(Methylsulfonyl)phenyl)methanamine	HCID 2760937	—
反応物	4-Carboxy-3-fluorophenylboronic acid	HCID 2763201	—
溶媒	Water	HCID 962	—
溶媒	Dimethylformamide	HCID 6228	—
生成物	HCID 123681539	HCID 123681539	88.3%

反応手順

A mixture of 4-borono-2-fluorobenzoic acid (218 mg, 1.2 mmol), (3-(methylsulfonyl)phenyl)-methanamine (200 mg, 1.08 mmol), DIEA (0.754 mL, 4.32 mmol) and TBTU (381 mg, 1.2 mmol) in DMF (2 mL) was stirred at room temperature for 2 days, then the reaction mixture was diluted with water (10 mL), and product precipitated out as gum, and the supernatant was separated via centrifugation, and the gummy residue was sonicated with water (3 mL), and the gummy residue was further dried under high vacuum yielding 3-fluoro-4-(3-(methylsulfonyl)benzylcarbamoyl)-phenylboronic acid (335 mg, 88%) as white foam. LCMS (m/z): 352.1 (MH+), 0.51 min.

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US09242996B2
出典データセット	uspto-grants-2016_01
ORD ID	ord-3417773766be496d8412b0b4494e335c
出典メモ	uspto-grants-2016_01