Acetic Acid → 2-(4'-((3aR,6aR)-hexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl)biphenyl-4-yl)pyridazin-3(2H)-one

참여 물질

역할	이름	HCID	투입량
반응물	Acetic Acid	HCID 176	—
반응물	(3aR,6aR)-ethyl 1-(4'-(6-oxopyridazin-1(6H)-yl)biphenyl-4-yl)hexahydropyrrolo[3,4-b]pyrrole-5(1H)-carboxylate	HCID 67396526	—
용매	Hydrogen Bromide	HCID 260	—
용매	Methanol	HCID 887	—
생성물	2-(4'-((3aR,6aR)-hexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl)biphenyl-4-yl)pyridazin-3(2H)-one	HCID 67396327	116.1%

반응 조건

온도	67.5 °C

반응 단계

A mixture of the product of Example 1E (7.50 g, 17.42 mmol) in 33% HBr in acetic acid (37 mL, 205.57 mmol, 11.8 equivalents) was heated to 65-70° C. for at least 6 hours while monitored by HPLC analysis for completion. When reaction is complete, the mixture is cooled to not more than 45° C. and is diluted with MeOH (111 mL). The mixture was cooled to 20-25° C., the product is collected by filtration and is washed with fresh MeOH (50 mL). The wet cake is dried in the vacuum oven at not more than 55° C. to provide the title compound (7.25 g, 94.8%).

출처 및 근거

DOI	10.6084/m9.figshare.5104873.v1
특허 번호	US08026240B2
출처 데이터셋	uspto-grants-2011_09
ORD ID	ord-65544bca844e4db5a601019f5e484df9
출처 메모	uspto-grants-2011_09