Acetic Acid → HCID 22707841, compound

HRID 353330Notes

Reaction equation

HRID 353330 reaction equation
[OH:1][NH:2][C:3]([C:5]1([S:15]([C:18]2[CH:23]=[CH:22][C:21]([O:24][C:25]3[CH:30]=[CH:29][C:28]([O:31][C:32]([F:35])([F:34])[F:33])=[CH:27][CH:26]=3)=[CH:20][CH:19]=2)(=[O:17])=[O:16])[CH2:10][CH2:9][N:8]([CH2:11][CH2:12][O:13][CH3:14])[CH2:7][CH2:6]1)=[O:4].[C:36]([OH:39])(=[O:38])[CH3:37]>C(OCC)(=O)C>[C:36]([OH:39])(=[O:38])[CH3:37].[OH:1][NH:2][C:3]([C:5]1([S:15]([C:18]2[CH:23]=[CH:22][C:21]([O:24][C:25]3[CH:26]=[CH:27][C:28]([O:31][C:32]([F:35])([F:33])[F:34])=[CH:29][CH:30]=3)=[CH:20][CH:19]=2)(=[O:17])=[O:16])[CH2:6][CH2:7][N:8]([CH2:11][CH2:12][O:13][CH3:14])[CH2:9][CH2:10]1)=[O:4]

Participants

4

Reactant 2

HCID 176Acetic AcidHCID 9892815HCID 9892815, compound

Product 1

HCID 22707841HCID 22707841, compoundYield 89%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

Part A: To a solution of Example 252 (0.5 g, 0.9 mmol) in ethyl acetate (5 mL) was added concentrated acetic acid (63.7 mg, 1.08 mmol) and solution was stirred at ambient temperature for 2 hours. Evaporation of the solvent and recrystallization from hot ethyl acetate gave the title compound as a white crystalline solid (0.4635 g, 83.0%). Analytical calculation for C22H25N2O7SF3.0.7C2H4O2: C, 50.14; H, 5.00; N, 5.00; S, 5.72. Found: C, 50.47; H, 5.09; N, 5.00; S, 6.13.

Workup

  1. customEvaporation of the solvent and recrystallization from hot ethyl acetate

Sources & evidence

ORD record
ord-90bd9ae9dbaf47f58090d309da21f84d
Source dataset
uspto-grants-2004_06
Patent number
US06750228B1

Reaction notes

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