Calcium Acetate → HCID 67451161, compound

HRID 1854792Notes

Reaction equation

HRID 1854792 reaction equation
[CH3:1][C:2]1[O:6][C:5]([C:7]([NH:9][C:10]([C:13]2[N:19]([CH3:20])[C:17](=[O:18])[C:16]([OH:21])=[C:15]([C:22]([NH:24][CH2:25][C:26]3[CH:27]=[CH:28][C:29]([F:32])=[CH:30][CH:31]=3)=[O:23])[N:14]=2)([CH3:12])[CH3:11])=[O:8])=[N:4][N:3]=1.C([O-])(=O)C.[Ca+2:37].C([O-])(=O)C.CCCCCCC>C(O)C.O>[CH3:1][C:2]1[O:6][C:5]([C:7]([NH:9][C:10]([C:13]2[N:19]([CH3:20])[C:17](=[O:18])[C:16]([OH:21])=[C:15]([C:22]([NH:24][CH2:25][C:26]3[CH:27]=[CH:28][C:29]([F:32])=[CH:30][CH:31]=3)=[O:23])[N:14]=2)([CH3:12])[CH3:11])=[O:8])=[N:4][N:3]=1.[Ca:37]

Participants

6

Reactant 3

HCID 6116Calcium AcetateHCID 8900Heptane2×HCID 54671008Raltegravir

Product 1

HCID 67451161HCID 67451161, compoundYield 90.8%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Conditions

Temperature
67.5 °C

Procedure

Raltegravir (10 gm) was suspended in ethanol (60 ml) and then added a solution of calcium acetate (4 gm) in water (2 ml) at 25 to 30° C. The contents were heated to 65 to 70° C. and distilled off solvent completely under vacuum at 45° C. to obtain residue. To the residue was added n-heptane (50 ml) and again distilled to obtain residue. n-Heptane (100 ml) was added to the residue and stirred for 6 hours at room temperature. The solid obtained was collected by filtration and dried to obtain 9.9 gm of raltegravir calcium.

Workup

  1. distillationdistilled off solvent completely under vacuum at 45° C.
  2. customto obtain residue
  3. distillationagain distilled
  4. customto obtain residue
  5. customThe solid obtained
  6. filtrationwas collected by filtration
  7. customdried

Sources & evidence

ORD record
ord-fca127ba780c4806aae357dab708cf25
Source dataset
uspto-grants-2015_02
Patent number
US08962833B2

Reaction notes

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