Acetic Anhydride → HCID 13936577, compound

HRID 2309273Notes

Reaction equation

HRID 2309273 reaction equation
[CH2:1]([N:8]1[N:12]=[N:11][C:10]([C:13]2[N:14]([CH3:26])[S:15](=[O:25])(=[O:24])[C:16]3[CH:23]=[CH:22][CH:21]=[CH:20][C:17]=3[C:18]=2[OH:19])=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:27](OC(=O)C)(=[O:29])[CH3:28]>>[C:27]([O:19][C:18]1[C:17]2[CH:20]=[CH:21][CH:22]=[CH:23][C:16]=2[S:15](=[O:25])(=[O:24])[N:14]([CH3:26])[C:13]=1[C:10]1[N:11]=[N:12][N:8]([CH2:1][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[N:9]=1)(=[O:29])[CH3:28]

Participants

3

Reactant 2

HCID 7918Acetic AnhydrideHCID 135838380HCID 135838380, compound

Product 1

HCID 13936577HCID 13936577, compoundYield 90.5%

Procedure

A mixture of compound (a) above (0.30 g) and acetic anhydride (5 ml) was refluxed for 4 hours and then concentrated. The residual oil solidified upon addition of n-hexane. After removal of the solvent by decantation, the solid was crystallized from toluene, filtered off and dried in vacuo to give 0.275 g (90.5%) of the title compound.

Workup

  1. temperaturewas refluxed for 4 hours
  2. concentrationconcentrated
  3. additionThe residual oil solidified upon addition of n-hexane
  4. customAfter removal of the solvent by decantation
  5. customthe solid was crystallized from toluene
  6. filtrationfiltered off
  7. customdried in vacuo

Sources & evidence

ORD record
ord-c8cdbdd0aa364e8f8eb0dd683c17dbe8
Source dataset
uspto-grants-1987_09
Patent number
US04694080

Reaction notes

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