Methanesulfonic Acid → HCID 131727723, compound

HRID 1432723Notes

Reaction equation

HRID 1432723 reaction equation
[CH2:1]([CH:3]([C:6]1[C:7]2[N:8]([C:13]([C:17]3[S:21][C:20]([N:22]([CH3:24])[CH3:23])=[N:19][C:18]=3[Cl:25])=[C:14]([CH3:16])[N:15]=2)[N:9]=[C:10]([CH3:12])[CH:11]=1)[CH2:4][CH3:5])[CH3:2].[CH3:26][S:27]([OH:30])(=[O:29])=[O:28]>C(OC(=O)C)C>[S:27]([OH:30])(=[O:29])(=[O:28])[CH3:26].[CH2:1]([CH:3]([C:6]1[C:7]2[N:8]([C:13]([C:17]3[S:21][C:20]([N:22]([CH3:23])[CH3:24])=[N:19][C:18]=3[Cl:25])=[C:14]([CH3:16])[N:15]=2)[N:9]=[C:10]([CH3:12])[CH:11]=1)[CH2:4][CH3:5])[CH3:2]

Participants

4

Reactant 2

HCID 6395Methanesulfonic AcidHCID 57933012HCID 57933012, compound

Product 1

HCID 131727723HCID 131727723, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

89 mg of N-{5-[8-(1-Ethyl-propyl)-2,6-dimethyl-imidazo[1,2-b]pyridazin-3-yl]-4-chloro-thiazol-2-yl}-dimethylamine (0.236 mmol) is dissolved in 2.0 ml of ethylacetate and 0.236 ml of 1M methanesulfonic acid in ethylacetate (0.236 mmol) is added. The solvents are removed under N2 gas and precipitated crystals are collected, washed with Et2O and dried. 92 mg (83%); mass spectrum (m/e): 378 (M+1); 1H-NMR (CDCl3): 7.30 (s, 1H), 3.67 (m, 1H), 3.22 (s, 6H), 2.93 (s, 3H), 2.78 (s, 3H), 2.78 (s, 3H), 2.71 (s, 3H), 1.95 (m, 2H), 1.82 (m, 2H), 0.96 (t, 6H, J=7.3 Hz).

Workup

  1. customThe solvents are removed under N2 gas
  2. customprecipitated crystals
  3. customare collected
  4. washwashed with Et2O
  5. customdried

Sources & evidence

ORD record
ord-3bb3694bf7044004bf98887738a49272
Source dataset
uspto-grants-2009_11
Patent number
US07612067B2

Reaction notes

Loading…