Phosphoric Acid → HCID 88028514, compound

HRID 353329Notes

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]>>[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

Reactant 2

HCID 1004Phosphoric Acid

HCID 9892815HCID 9892815, compound

Product 1

HCID 88028514HCID 88028514, compoundYield 88.6%

Procedure

Part A: To the ethyl acetate solution (4 mL) of Example 252 (0.5 g, 0.9 mmol) was added concentrated phosphoric acid (85%, 0.1248 g, 1.08 mmol) and solution was stirred at ambient temperature for 2 hours. Evaporation of the solvent and recrystallization from hot ethanol gave the title compound as a white powder (0.4917 g, 82.7%). Analytical calculation for C22H25N2O7SF3.H3PO4.H2O: C, 41.64; H, 4.77; N, 4.42. Found: C, 41.14; H, 4.64; N, 4.25.

Workup

customEvaporation of the solvent and recrystallization from hot ethanol

Sources & evidence

ORD record: ord-b41c81cb6c3e4aaf95a0b4d9e38c7042
Source dataset: uspto-grants-2004_06
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06750228B1

Reaction notes

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