Dichloromethane → HCID 67202227, compound

HRID 1921092Notes

Reaction equation

HRID 1921092 reaction equation
[CH3:1][CH2:2][O:3][C:4]([N:6]1[C:21]([NH2:22])=[C:9]2[CH2:10][N:11](C(OC(C)(C)C)=O)[CH2:12][CH2:13][C:8]2=[N:7]1)=[O:5].O1CCOCC1.[Cl:29]CCl>Cl>[ClH:29].[CH2:2]([O:3][C:4]([N:6]1[C:21]([NH2:22])=[C:9]2[CH2:10][NH:11][CH2:12][CH2:13][C:8]2=[N:7]1)=[O:5])[CH3:1]

Participants

5

Reactant 3

HCID 6344DichloromethaneHCID 312751,4-DioxaneHCID 67200254HCID 67200254, compound

Product 1

HCID 67202227HCID 67202227, compoundYield 99%

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent

Procedure

To a solution of 3-amino-6,7-dihydro-4H-pyrazolo[4,3-c]pyridine-2,5-dicarboxylic acid 5-tert-butyl ester 2-ethyl ester (40 g, 128.9 mmol) in dichloromethane (1 L), 4 N HCl in dioxane (161 mL, 644.5 mmol) was added dropwise. The mixture was stirred at room temperature for 4 hours. The solid was filtered, washed with dichloromethane and diethylether. After drying in vacuo the title compound was obtained as white solid (36.2 g, 99%).

Workup

  1. filtrationThe solid was filtered
  2. washwashed with dichloromethane and diethylether
  3. dry with materialAfter drying in vacuo the title compound

Sources & evidence

ORD record
ord-16f1fc495cc5468fbfe3f731ec43f985
Source dataset
uspto-grants-2012_05
Patent number
US08173659B2

Reaction notes

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