Methylamine → HCID 23284693, compound

HRID 369292Notes

Reaction equation

HRID 369292 reaction equation
[CH3:1][NH2:2].[NH2:3][C:4]1[C:5]([F:29])=[CH:6][C:7]([F:28])=[C:8]([N:10]2[C:19]3[C:14](=[CH:15][C:16]([F:23])=[C:17](F)[C:18]=3[CH2:20][OH:21])[C:13](=[O:24])[C:12]([C:25]([OH:27])=[O:26])=[CH:11]2)[CH:9]=1>N1C=CC=CC=1>[NH2:3][C:4]1[C:5]([F:29])=[CH:6][C:7]([F:28])=[C:8]([N:10]2[C:19]3[C:14](=[CH:15][C:16]([F:23])=[C:17]([NH:2][CH3:1])[C:18]=3[CH2:20][OH:21])[C:13](=[O:24])[C:12]([C:25]([OH:27])=[O:26])=[CH:11]2)[CH:9]=1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 23284669HCID 23284669, compound

Product 1

HCID 23284693HCID 23284693, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Conditions

Temperature
40 °C

Procedure

Pyridine (300 mg) and a 40% aqueous solution (150 mg) of methylamine were added to 1(5-amino-2,4-difluorophenyl)-6,7-difluoro-8-hydroxymethyl-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (100 mg), and the mixture was stirred overnight at 40° C. The solvent and the like were distilled off, and diethyl ether was added to the residue. A supernatant liquid was removed, and ethanol was added to the resultant residue. Solids deposited were collected by filtration to obtain the title compound (34 mg) as a yellow powder.

Workup

  1. distillationThe solvent and the like were distilled off
  2. additiondiethyl ether was added to the residue
  3. customA supernatant liquid was removed
  4. additionethanol was added to the resultant residue
  5. filtrationSolids deposited were collected by filtration

Sources & evidence

ORD record
ord-abe3dc9581ce48d2a42b3eabb74aec32
Source dataset
uspto-grants-2000_10
Patent number
US06136823

Reaction notes

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