Acetonitrile → N-(2-Fluoro-benzyl)-2-methyl-N'-(5-methyl-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl)-malonamide

참여 물질

역할	이름	HCID	투입량
반응물	Acetonitrile	HCID 6342	—
반응물	2-Fluorobenzylamine	HCID 66649	—
반응물	O-(2-Oxo-1(2H)-pyridyl)-N,N,N',N'-tetramethyluronium Tetrafluoroborate	HCID 2733204	—
반응물	2-Methyl-N-(5-methyl-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl)-malonamic acid	HCID 21072500	—
용매	Dimethylformamide	HCID 6228	—
용매	Trifluoroacetic acid	HCID 6422	—
생성물	N-(2-Fluoro-benzyl)-2-methyl-N'-(5-methyl-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl)-malonamide	HCID 10095038	—

반응 단계

2-Methyl-N-(5-methyl-6-oxo-6,7-dihydro-5H-dibenzo[b,d]azepin-7-yl)-malonamic acid (20 mg, 0.059 mmol) and 2-fluorobenzylamine (7.4 mg, 0.059 mmol) were placed in a disposable polypropylene tube and dissolved in DMF (2 ml). TPTU (2-(2-pyridon-1-yl)-1,1,3,3-tetramethyl uronium tetrafluoroborate, 19 mg, 0.065 mmol) was added, and the mixture was shaken overnight at r.t. The title compound, MS: m/e=446.2 (M+H+), was isolated from the reaction mixture by automated, preparative HPLC (YMC CombiPrep C18 column 50×20 mm, solvent gradient 5-95% CH3CN in 0.1% TFA(aq) over 6.0 min, λ=230 nm, flow rate 40 ml/min).

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US07375099B2
출처 데이터셋	uspto-grants-2008_05
ORD ID	ord-098052cde1b646a8a419eee7f045e41f
출처 메모	uspto-grants-2008_05