Hydrochloric Acid → HCID 136375765, compound

HRID 869265Notes

Reaction equation

HRID 869265 reaction equation
[C:1]([C:4]1[C:9](=[O:10])[NH:8][C:7]([NH:11][CH:12]2[CH2:17][CH2:16][CH2:15][N:14](C(OC(C)(C)C)=O)[CH2:13]2)=[N:6][C:5]=1[NH:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][C:27]=1[S:32]([CH:35]([CH3:37])[CH3:36])(=[O:34])=[O:33])(=[O:3])[NH2:2].[ClH:38]>C(OCC)(=O)C>[ClH:38].[ClH:38].[CH:35]([S:32]([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][C:26]=1[NH:25][C:5]1[N:6]=[C:7]([NH:11][CH:12]2[CH2:17][CH2:16][CH2:15][NH:14][CH2:13]2)[NH:8][C:9](=[O:10])[C:4]=1[C:1]([NH2:2])=[O:3])(=[O:34])=[O:33])([CH3:37])[CH3:36]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 136375760HCID 136375760, compound

Product 1

HCID 136375765HCID 136375765, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

To a mixture of tert-butyl 3-[(5-carbamoyl-4-{[2-(isopropylsulfonyl)phenyl]amino}-6-oxo-1,6-dihydropyrimidine-2-yl)amino]piperidine-1-carboxylate (Example 28) (299 mg) and ethyl acetate (3 mL), 4M hydrogen chloride in ethyl acetate (2.7 mL) was added under ice cooling and stirred at room temperature for 1 hour. The precipitated solid was collected by filtration and dried to give 4-{[2-(isopropylsulfonyl)phenyl]amino}-6-oxo-2-(piperidin-3-ylamino)-1,6-dihydropyrimidine-5-carboxamide dihydrochloride (194 mg) as a white solid.

Workup

  1. additionwas added under ice cooling
  2. filtrationThe precipitated solid was collected by filtration
  3. customdried

Sources & evidence

ORD record
ord-67a9f9b09abf49a081f0257a4c41b0ac
Source dataset
uspto-grants-2015_03
Patent number
US08969336B2

Reaction notes

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