Methylamine → HCID 86756619, compound

HRID 324495Notes

Reaction equation

HRID 324495 reaction equation
Cl[C:2]1[S:3][C:4]2[CH:11]=[CH:10][C:9]3[CH:12]=[C:13]([Cl:16])[CH:14]=[CH:15][C:8]=3[CH:7]([C:17]3[C:18](=[O:25])[NH:19][C:20](=[O:24])[N:21]([CH3:23])[CH:22]=3)[C:5]=2[N:6]=1.[CH3:26][NH2:27]>C(O)C>[Cl:16][C:13]1[CH:14]=[CH:15][C:8]2[CH:7]([C:17]3[C:18](=[O:25])[NH:19][C:20](=[O:24])[N:21]([CH3:23])[CH:22]=3)[C:5]3[N:6]=[C:2]([NH:27][CH3:26])[S:3][C:4]=3[CH:11]=[CH:10][C:9]=2[CH:12]=1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 70113243(+/-)-5-(2,7-Dichloro-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-1-methyl-2,4(1H,3H)-pyrimidinedione

Product 1

HCID 86756619HCID 86756619, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

The product from example 44 step (viii) (0.05 g) was heated with 40% aq. Methylamine (4 ml) in ethanol (1 ml) for 3 hours. The mixture was partitioned between ethyl acetate and water. The organic phase was collected, dried (MgSO4) and solvent evaporated under reduced pressure. The residue was triturated with ethyl acetate/iso-hexane mixtures and the title product collected by filtration as a pale yellow solid.

Workup

  1. customThe mixture was partitioned between ethyl acetate and water
  2. customThe organic phase was collected
  3. dry with materialdried (MgSO4) and solvent
  4. customevaporated under reduced pressure
  5. customThe residue was triturated with ethyl acetate/iso-hexane mixtures
  6. filtrationthe title product collected by filtration as a pale yellow solid

Sources & evidence

ORD record
ord-704be0583aca46c18803d136c4229b03
Source dataset
uspto-grants-2001_04
Patent number
US06218376B1

Reaction notes

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