Hydrochloric Acid → HCID 135673971, compound

HRID 393905Notes

Reaction equation

HRID 393905 reaction equation
[ClH:1].[C:2]([C:5]1[CH:6]=[C:7]([C:16]2[NH:17][C:18](=[O:33])[C:19]3[C:20](=[C:22]([CH2:31][CH3:32])[N:23]([CH:25]4[CH2:28][N:27]([CH2:29][CH3:30])[CH2:26]4)[N:24]=3)[N:21]=2)[C:8]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])=[N:9][CH:10]=1)(=[O:4])[CH3:3]>O1CCOCC1.C(OCC)(=O)C>[ClH:1].[C:2]([C:5]1[CH:6]=[C:7]([C:16]2[NH:17][C:18](=[O:33])[C:19]3[C:20](=[C:22]([CH2:31][CH3:32])[N:23]([CH:25]4[CH2:28][N:27]([CH2:29][CH3:30])[CH2:26]4)[N:24]=3)[N:21]=2)[C:8]([O:11][CH2:12][CH2:13][CH2:14][CH3:15])=[N:9][CH:10]=1)(=[O:4])[CH3:3]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 1355155655-(5-acetyl-2-butoxy-3-pyridinyl)-3-ethyl-2-(1-ethyl-3-azetidinyl)-2,6-dihydro-7H-pyrazolo(4,3-d)pyrimidin-7-one

Product 1

HCID 135673971HCID 135673971, compound

Reagents, catalysts & solvents 2

HCID 8857Ethyl AcetateSolvent2×HCID 312751,4-DioxaneSolvent

Conditions

Temperature
50 °C

Procedure

A solution of 4M hydrochloric acid in dioxan (1 mL) was added to ethyl acetate (3 mL). An aliquot of this solution (0.3 mL), was then added to a solution of 5-(5-acetyl-2-butoxy-3-pyridinyl)-3-ethyl-2-(1-ethyl-3-azetidinyl)-2,6-dihydro-7H-pyrazolo[4,3-d]pyrimidin-7-one (132 mg, 0.3 mmol) in ethyl acetate (5 mL) giving a precipitate. This mixture was warmed to 50° C. for 10 minutes, then allowed to cool to 0° C. The resulting powder was filtered, washed with ethyl acetate and dried at 50° C. in vacuo, to afford the title compound, 118 mg (81%).

Workup

  1. customgiving a precipitate
  2. temperatureto cool to 0° C
  3. filtrationThe resulting powder was filtered
  4. washwashed with ethyl acetate
  5. customdried at 50° C. in vacuo

Sources & evidence

ORD record
ord-1887041d39564e879a62a73f588946ef
Source dataset
uspto-grants-2004_10
Patent number
US06809200B2

Reaction notes

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