Acetic Anhydride → HCID 69050511, compound

HRID 1784112Notes

Reaction equation

HRID 1784112 reaction equation
[NH2:1][C:2]1([NH2:23])[NH:11][C:10](=[O:12])[C:9]2[C:4](=[N:5][CH:6]=[C:7]([C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([O:21][CH3:22])[CH:14]=3)[N:8]=2)[NH:3]1.[C:24](OC(=O)C)(=[O:26])[CH3:25]>C(O)(=O)C>[C:24]([NH:23][C:2]1([NH2:1])[NH:11][C:10](=[O:12])[C:9]2[C:4](=[N:5][CH:6]=[C:7]([C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[C:15]([O:21][CH3:22])[CH:14]=3)[N:8]=2)[NH:3]1)(=[O:26])[CH3:25]

Participants

4

Reactant 2

HCID 7918Acetic AnhydrideHCID 69048812HCID 69048812, compound

Product 1

HCID 69050511HCID 69050511, compoundYield 77%

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A suspension of the compound of example 48 (10.46 g, 35 mmoles) in acetic anhydride (600 ml) and acetic acid (200 ml) was refluxed for 1 hour until a clear solution was formed. By cooling down the reaction mixture in the refrigerator, the precipitate formed was filtered off, washed with ethyl acetate and diethyl ether, and then dried over P2O5 under vacuum, providing the title compound as a yellow powder (9.19 g, yield: 77%). This compound was further characterized by the following spectra:

Workup

  1. temperaturewas refluxed for 1 hour until a clear solution
  2. customwas formed
  3. temperatureBy cooling down the reaction mixture in the refrigerator
  4. customthe precipitate formed
  5. filtrationwas filtered off
  6. washwashed with ethyl acetate and diethyl ether
  7. dry with materialdried over P2O5 under vacuum

Sources & evidence

ORD record
ord-42095b2608ea4e5298f1660f83f003b0
Source dataset
uspto-grants-2009_03
Patent number
US07501513B2

Reaction notes

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