Methanol → HCID 18957862, compound

HRID 2379073Notes

Reaction equation

HRID 2379073 reaction equation
C[O:2][C:3]([C:5]1[CH:10]=[CH:9][C:8](=[O:11])[N:7]([CH2:12][CH2:13][NH:14][C:15]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][N:18]=2)=[O:16])[CH:6]=1)=[O:4].CO.O.C(=O)([O-])[O-].[Na+].[Na+]>C(O)(=O)C>[N:18]1[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=1[C:15]([NH:14][CH2:13][CH2:12][N:7]1[C:8](=[O:11])[CH:9]=[CH:10][C:5]([C:3]([OH:4])=[O:2])=[CH:6]1)=[O:16]

Participants

6

Reactant 4

HCID 887MethanolHCID 962WaterHCID 10340Sodium CarbonateHCID 9904451HCID 9904451, compound

Product 1

HCID 18957862HCID 18957862, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
60 °C

Procedure

To a 10 ml round bottomed flask fitted with a magnetic stirrer bar was added 1,6-dihydro-1-[2-(2-pyridinylcarbonylamino)ethyl]-6-oxo-3-pyridinecarboxylic acid methyl ester (0.177 g, 0.59 mmol), methanol (1.4 ml), water (1.4 ml), and 15% aqueous sodium carbonate (1.4 ml). The resulting suspension was heated in a 60° C. oil bath for 1 hour during which time the mixture was completely solvated. Upon cooling to room temperature, acetic acid was added dropwise, with stirring, to a final pH of 5.5. The precipitated product was recovered by filtration, washed with water, and dried at 50° C. under high vacuum, MP: 266°-268° C.

Workup

  1. customTo a 10 ml round bottomed flask fitted with a magnetic stirrer bar
  2. temperatureUpon cooling to room temperature
  3. filtrationThe precipitated product was recovered by filtration
  4. washwashed with water
  5. customdried at 50° C. under high vacuum, MP: 266°-268° C.

Sources & evidence

ORD record
ord-2af0eaa68c424b6fbcc6aace5a68e320
Source dataset
uspto-grants-1994_11
Patent number
US05360808

Reaction notes

Loading…