Oxalic Acid → HCID 86753237, compound

HRID 1870990Notes

Reaction equation

HRID 1870990 reaction equation
[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[CH3:7][C:8]1[O:32][C:11]2=[C:12]3[O:17][CH:16]([CH2:18][NH:19][CH2:20][CH2:21][CH2:22][NH:23][C:24]4[N:29]=[CH:28][CH:27]=[CH:26][N:25]=4)[CH2:15][CH2:14][C:13]3=[CH:30][CH:31]=[C:10]2[C:9]=1[CH3:33].C(O)(=O)C(O)=O>C(Cl)Cl.CO>[C:1]([OH:6])(=[O:5])[C:2]([OH:4])=[O:3].[N:25]1[CH:26]=[CH:27][CH:28]=[N:29][C:24]=1[NH:23][CH2:22][CH2:21][CH2:20][NH:19][CH2:18][CH:16]1[CH2:15][CH2:14][C:13]2=[CH:30][CH:31]=[C:10]3[CH:9]([CH3:33])[CH:8]([CH3:7])[O:32][C:11]3=[C:12]2[O:17]1

Participants

4

Reactant 2

HCID 971Oxalic AcidHCID 131720891HCID 131720891, compound

Product 1

HCID 86753237HCID 86753237, compoundYield 3.3%

Reagents, catalysts & solvents 1

HCID 21226129Dichloromethane methanolSolvent

Procedure

CH2Cl2 /CH3OH 85/15). The desired fractions were collected and the solvent was evaporated. The residue (1.8 g) was dissolved in ethanol and converted into the ethanedioic acid salt (1:2) with ethanedioic acid (0.010 mol). The precipitate was filtered off and dried, yielding 1.1 g (3.3%) (±)-N-2-pyrimidinyl-N'-[(3,6,7,8-tetrahydro-2,3-dimethyl-2H-furo[3,2-h][1]benzopyran-8-yl)methyl]-1,3-propanediamine ethanedioate(1:2); mp. 171.2° C. (comp. 8-a).

Workup

  1. customThe desired fractions were collected
  2. customthe solvent was evaporated
  3. dissolutionThe residue (1.8 g) was dissolved in ethanol
  4. filtrationThe precipitate was filtered off
  5. customdried

Sources & evidence

ORD record
ord-2fe5e208ba684d1d8cf9bc64e6add1bb
Source dataset
uspto-grants-2000_08
Patent number
US06100268

Reaction notes

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