Oxalic acid dihydrate → HCID 178443391, compound

HRID 1437074Notes

Reaction equation

HRID 1437074 reaction equation
C(O)(=O)C.[CH3:5][C:6]1([CH3:33])[N:11]=[C:10]([NH:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)[NH:9][C:8]([NH:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])=[N:7]1.O.O.[C:36]([OH:41])(=[O:40])[C:37]([OH:39])=[O:38]>C(#N)C>[C:36]([OH:41])(=[O:40])[C:37]([OH:39])=[O:38].[CH3:5][C:6]1([CH3:33])[N:11]=[C:10]([NH:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)[NH:9][C:8]([NH:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH3:32])=[N:7]1

Participants

4

Reactant 2

HCID 61373Oxalic acid dihydrateHCID 178476233HCID 178476233, compound

Product 1

HCID 178443391HCID 178443391, compoundYield 36.4%

Reagents, catalysts & solvents 1

HCID 6342AcetonitrileSolvent

Procedure

6.5 g (16.2 mmol) of the compound (1) of Working Example 38 was dissolved in 50 ml of 30% aqueous acetonitrile, and 3.0 g (23.8 mmol) of oxalic acid dihydrate was added thereto. The mixture was dissolved under heating, and then cooled. The resulting crystals were recrystallized from 50% aqueous acetonitrile to obtain 2.9 g of colorless crystals having a melting point of 101 to 103° C.

Workup

  1. dissolutionThe mixture was dissolved
  2. temperatureunder heating
  3. temperaturecooled
  4. customThe resulting crystals were recrystallized from 50% aqueous acetonitrile

Sources & evidence

ORD record
ord-bcaeb2ad11694585b07924d20a9fd4b0
Source dataset
uspto-grants-2009_11
Patent number
US07622469B2

Reaction notes

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