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 1947419Notes

Reaction equation

HRID 1947419 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]>CO>[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

4

Reactant 2

HCID 313Hydrochloric AcidHCID 24743471Abt-288

Product 1

HCID 247439162-{4'-[(3aR,6aR)-5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl]-1,1'-biphenyl-4-yl}pyridazin-3(2H)-one HCl

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent2×

Procedure

2-{4′-[(3aR,6aR)-5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl]-1,1-biphenyl-4-yl}pyridazin-3(2H)-one (226 mg) was suspended in methanol (4.0 mL). A solution of 1 M HCl in methanol (0.66 mL) was added to the suspension dropwise. Throughout the process the suspension is stirred using a magnetic stirrer. Most of the solid dissolved leaving a light suspension. Upon sonication, crystallization was observed. The resulting suspension was agitated at ambient temperatures overnight before the crystals were harvested.

Workup

  1. dissolutionMost of the solid dissolved
  2. customleaving a light suspension
  3. customUpon sonication, crystallization
  4. stirringThe resulting suspension was agitated at ambient temperatures overnight before the crystals

Sources & evidence

ORD record
ord-df6f87bdd9274df5af8e320e25c38303
Source dataset
uspto-grants-2013_03
Patent number
US08399468B2

Reaction notes

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