Hydrochloric Acid → 2-{4'-[(3aR,6aR)-5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl]-1,1'-biphenyl-4-yl}pyridazin-3(2H)-one HCl

HRID 12984

Reaction equation

[CH3:1][N:2]1[CH2:9][C@@H:8]2[C@@H:4]([N:5]([C:10]3[CH:15]=[CH:14][C:13]([C:16]4[CH:21]=[CH:20][C:19]([N:22]5[C:27](=[O:28])[CH:26]=[CH:25][CH:24]=[N:23]5)=[CH:18][CH:17]=4)=[CH:12][CH:11]=3)[CH2:6][CH2:7]2)[CH2:3]1.[ClH:29]>ClCCl>[ClH:29].[CH3:1][N:2]1[CH2:9][C@@H:8]2[C@@H:4]([N:5]([C:10]3[CH:15]=[CH:14][C:13]([C:16]4[CH:21]=[CH:20][C:19]([N:22]5[C:27](=[O:28])[CH:26]=[CH:25][CH:24]=[N:23]5)=[CH:18][CH:17]=4)=[CH:12][CH:11]=3)[CH2:6][CH2:7]2)[CH2:3]1

Participants

Conditions

Temperature: 50 °C

Procedure

2-{4′-[(3aR,6aR)-5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl]-1,1′-biphenyl-4-yl}pyridazin-3(2H)-one (372 mg) was suspended in dichloromethane (1.5 mL). The suspension was heated to about 50° C. A 1 M HCl (1.1 mL) solution was added to the suspension in dichloromethane dropwise. Throughout the process the suspension is stirred using a magnetic stirrer and temperature maintained at about 50° C. Most of the solid dissolved leaving a light suspension when about one third of the HCl solution was added. Upon further addition of the HCl solution, crystallization was observed. The resulting suspension was agitated at ambient temperatures overnight before the crystals were harvested.

Workup

temperaturetemperature maintained at about 50° C
dissolutionMost of the solid dissolved

Sources & evidence

ORD record: ord-8a15621959e84278bfaf15e6865856ef
Source dataset: uspto-grants-2010_06
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US07728031B2

Linked notes

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