Hydrochloric Acid → HCID 59007048, compound

HRID 130414Notes

Reaction equation

HRID 130414 reaction equation
[CH3:1][C@H:2]1[NH:7][C@@H:6]([CH3:8])[CH2:5][N:4]([C:9]2[C:10]([F:21])=[CH:11][C:12]([O:19][CH3:20])=[C:13]([NH:15]C(=O)C)[CH:14]=2)[CH2:3]1.Cl>C(O)C>[CH3:1][C@H:2]1[NH:7][C@@H:6]([CH3:8])[CH2:5][N:4]([C:9]2[C:10]([F:21])=[CH:11][C:12]([O:19][CH3:20])=[C:13]([CH:14]=2)[NH2:15])[CH2:3]1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 69198739HCID 69198739, compound

Product 1

HCID 59007048HCID 59007048, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of product from Step 3 (883 mg, 3 mmol) in ethanol (40 ml) containing concentrated hydrochloric acid (2 ml) was heated at reflux for 15 hours. After cooling, the mixture was purified using an SCX ion exchange cartridge (Varian bond-elute) eluting with methanol and then 2M ammonia in methanol. The appropriate basic fractions were reduced in vacuo to afford the title compound (D18). MS (ES+) m/e 254 [M+H]+.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 15 hours
  3. temperatureAfter cooling
  4. customthe mixture was purified
  5. washan SCX ion exchange cartridge (Varian bond-elute)
  6. washeluting with methanol

Sources & evidence

ORD record
ord-5f71489c6c784c54a4fca64732fa8f76
Source dataset
uspto-grants-2008_06
Patent number
US07381728B2

Reaction notes

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