Hydrochloric Acid → HCID 137220062, compound

HRID 1580976Notes

Reaction equation

HRID 1580976 reaction equation
[CH2:1]([N:3]1[C:7]2[NH:8][C:9](=[O:13])[CH2:10][CH:11]([CH3:12])[C:6]=2[C:5]([CH3:14])=[N:4]1)[CH3:2].C(O)C.[ClH:18]>CCOCC>[ClH:18].[CH2:1]([N:3]1[C:7]2[NH:8][C:9](=[O:13])[CH2:10][CH:11]([CH3:12])[C:6]=2[C:5]([CH3:14])=[N:4]1)[CH3:2]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 135783978HCID 135783978, compound

Product 1

HCID 137220062HCID 137220062, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

23.4 G. of 1-ethyl-1,4,5,7-tetrahydro-3,4-dimethyl6H-pyrazolo[3,4-b]pyridin-6-one (0.12 mol.) are dissolved in 70 ml. of absolute ethanol while warming. After cooling, 32 ml. of ethereal hydrochloric acid (0.2 mol.HCl/l) are added to the solution. Two hours later, 100 ml. of absolute ether are added and the mixture is let stand overnight. The crystallized 1-ethyl-1,4,5,7-tetrahydro-3,4-dimethyl-6H-pyrazolo[3,4-b]pyridin-6-one, hydrochloride is filtered off and dried at 50°, yield 25.3 g. (92%), m.p. 192°-195° (dec.).

Workup

  1. temperatureAfter cooling
  2. customTwo hours
  3. filtrationThe crystallized 1-ethyl-1,4,5,7-tetrahydro-3,4-dimethyl-6H-pyrazolo[3,4-b]pyridin-6-one, hydrochloride is filtered off
  4. customdried at 50°

Sources & evidence

ORD record
ord-d3b2e7a373994e959359265d4c61cf0d
Source dataset
uspto-grants-1976_01
Patent number
US03935222

Reaction notes

Loading…