Trifluoroacetic acid → HCID 18172498, compound

HRID 926551Notes

Reaction equation

HRID 926551 reaction equation
CC1(C)[O:7][C:6](=[O:8])[CH:5]([CH2:9][C:10]2[CH:11]=[C:12]([CH:15]=[CH:16][CH:17]=2)[C:13]#[N:14])[C:4](=[O:18])[O:3]1.C(O)(C(F)(F)F)=O.[O-]S([O-])(=O)=O.[Ca+2]>O>[C:13]([C:12]1[CH:11]=[C:10]([CH:17]=[CH:16][CH:15]=1)[CH2:9][CH:5]([C:4]([OH:18])=[O:3])[C:6]([OH:8])=[O:7])#[N:14]

Participants

5

Reactant 3

HCID 6422Trifluoroacetic acidHCID 24497Calcium SulfateHCID 23509302HCID 23509302, compound

Product 1

HCID 18172498HCID 18172498, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A flask containing a mixture of 3-((2,2-dimethyl-4,6-dioxo-1,3-dioxan-5-yl)methyl)benzonitrile (4.53 g, 17.5 mmol, Intermediate 70: step a) TFA (30 mL) and water (14 mL) was equipped with a reflux condenser and Drierite® at the outlet, then heated in a 65° C. oil bath for 4 hours. The mixture was concentrated and the title compound was precipitated from water and filtered.

Workup

  1. additionA flask containing
  2. concentrationThe mixture was concentrated
  3. customthe title compound was precipitated from water
  4. filtrationfiltered

Sources & evidence

ORD record
ord-f5062877a8b14ff7980c3895ba14dad2
Source dataset
uspto-grants-2016_03
Patent number
US09284308B2

Reaction notes

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