p-Toluenesulfonic acid monohydrate → 4-(9'-cyclopentyl-5'-methyl-6'-oxo-5',6',8',9'-tetrahydrospiro[cyclopropane-1,7'-pyrimido[5,4-b][1,4]diazepine]-2'-ylamino)-N-(1-ethyl-4-piperidyl)-3-fluoro-benzamide

참여 물질

역할	이름	HCID	투입량
반응물	p-Toluenesulfonic acid monohydrate	HCID 521998	—
반응물	4-amino-N-(1-ethylpiperidin-4-yl)-3-fluorobenzamide	HCID 55102782	—
반응물	2-chloro-9-cyclopentyl-8,9-dihydro-5-methylspiro[5H-pyrimido[4,5-b][1,4]diazepine-7,1'-cyclopropan]-6(7H)-one	HCID 57969939	—
용매	4-Methyl-2-Pentanol	HCID 7910	—
생성물	4-(9'-cyclopentyl-5'-methyl-6'-oxo-5',6',8',9'-tetrahydrospiro[cyclopropane-1,7'-pyrimido[5,4-b][1,4]diazepine]-2'-ylamino)-N-(1-ethyl-4-piperidyl)-3-fluoro-benzamide	HCID 68686234	—

반응 조건

온도	160 °C

반응 단계

2′-chloro-9′-cyclopentyl-5′-methyl-8′,9′-dihydrospiro[cyclopropane-1,7′-pyrimido[5,4-b][1,4]diazepin]-6′(5′H)-one (Intermediate 130; 231 mg, 0.75 mmol), 4-amino-N-(1-ethylpiperidin-4-yl)-3-fluorobenzamide (200 mg, 0.75 mmol) and p-toluenesulfonic acid monohydrate (335 mg, 1.88 mmol) were suspended in 4-Methyl-2-pentanol (5 mL) and sealed into a microwave tube. The reaction was heated to 160° C. for 30 minutes in the microwave reactor and allowed to cool to room temperature.

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US07709471B2
출처 데이터셋	uspto-grants-2010_05
ORD ID	ord-4696f7cafc21438e93b43739fd86f985
출처 메모	uspto-grants-2010_05