Phosphoric Acid → HCID 88028514, compound

HRID 353333Notes

Reaction equation

HRID 353333 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].[P:36](=[O:40])([OH:39])([OH:38])[OH:37]>C(OCC)(=O)C>[P:36]([OH:40])([OH:39])([OH:38])=[O: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 1004Phosphoric AcidHCID 9892815HCID 9892815, compound

Product 1

HCID 88028514HCID 88028514, compoundYield 158.2%

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 phosphoric acid (37 mg, 0.32 mmol) and solution was stirred at ambient temperature for 2 hours. Evaporation of the solvent and recrystallization from hot ethanol at zero degrees Celsius gave the title compound as a white solid (0.312 g, 59%). Analytical calculation for C22H25N2O7SF3.0.33H3PO4.0.5H2O: C, 47.18; H, 4.86; N, 5.00. Found: C, 47.15; H, 4.73; N, 4.90.

Workup

  1. customEvaporation of the solvent and recrystallization from hot ethanol at zero degrees Celsius

Sources & evidence

ORD record
ord-e0cd037645fb4c4187429668bedde3da
Source dataset
uspto-grants-2004_06
Patent number
US06750228B1

Reaction notes

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