HCID 68813464, compound → HCID 68813851, compound

HRID 2105225Notes

Reaction equation

HRID 2105225 reaction equation
ClC1C(NC2C=C(C)NN=2)=[N:4][C:5]([N:8]2[CH2:13][CH2:12][CH2:11]C[CH:9]2[C:14]2[O:18][N:17]=[C:16]([C:19]3[CH:24]=[CH:23]C=CN=3)[CH:15]=2)=[N:6]C=1>CO>[CH:19]1([C:16]2[CH:15]=[C:14]([CH:9]3[CH2:11][CH2:12][CH2:13][N:8]3[C:5](=[NH:4])[NH2:6])[O:18][N:17]=2)[CH2:24][CH2:23]1

Participants

3

Reactant 1

HCID 68813464HCID 68813464, compound

Product 1

HCID 68813851HCID 68813851, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
60 °C

Procedure

A mixture of 2-(3-cyclopropylisoxazol-5-yl)pyrrolidine (Method 14) (2.05 g, 11.5 mmol) and formamidinesulphonic acid (1.425 g, 11.5 mmol) in dry methanol (30 ml) was heated at 60° C. for 18 hours. The solvent was removed by evaporation and the residue dissolved in water. The aqueous solution was washed with water and then the water removed by evaporation. The residue was triturated with ether/DCM, the solid product was collected and dried under vacuum at 50° C. for 18 hours to give the title compound monosulphate salt (1.839 mg, 41%); m/z 221 [MH]+.

Workup

  1. customThe solvent was removed by evaporation
  2. dissolutionthe residue dissolved in water
  3. washThe aqueous solution was washed with water
  4. customthe water removed by evaporation
  5. customThe residue was triturated with ether/DCM
  6. customthe solid product was collected
  7. customdried under vacuum at 50° C. for 18 hours

Sources & evidence

ORD record
ord-cb02fb7affdf4ee4824886d348710d4e
Source dataset
uspto-grants-2009_08
Patent number
US07579349B2

Reaction notes

Loading…