Water → HCID 135422991, compound

HRID 1167061Notes

Reaction equation

HRID 1167061 reaction equation
[CH3:1][C:2]1[S:6][C:5]2[NH:7][C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=3[N:14]=[C:15]([N:16]3[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]3)[C:4]=2[CH:3]=1.[OH2:23]>C(OCC)(=O)C.C1(C)C=CC=CC=1>[OH2:23].[OH2:23].[CH3:1][C:2]1[S:6][C:5]2[NH:7][C:8]3[CH:9]=[CH:10][CH:11]=[CH:12][C:13]=3[N:14]=[C:15]([N:16]3[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]3)[C:4]=2[CH:3]=1

Participants

5

Reactant 2

HCID 962WaterHCID 135398745Olanzapine

Product 1

HCID 135422991HCID 135422991, compound

Reagents, catalysts & solvents 2

HCID 1140TolueneSolventHCID 8857Ethyl AcetateSolvent

Conditions

Temperature
80 °C

Procedure

A 0.5 g sample of technical grade olanzapine was suspended in ethyl acetate (10 mL) and toluene (0.6 mL). The mixture was heated to 80° C. until all the solids dissolved. The solution was cooled to 60° C. and water (1 mL) was added slowly. As the solution cooled to room temperature, a crystal slurry formed. The product was isolated using vacuum filtration and dried under ambient conditions. The product was identified as Dihydrate E using x-ray powder analysis and solid state 13C NMR. TGA mass loss was 10.5%. Yield: 0.3 g.

Workup

  1. dissolutiondissolved
  2. temperatureThe solution was cooled to 60° C.
  3. temperatureAs the solution cooled to room temperature
  4. customa crystal slurry formed
  5. customThe product was isolated
  6. filtrationvacuum filtration
  7. customdried under ambient conditions

Sources & evidence

ORD record
ord-08dbf98ea9de4216a57d3c19b5b23e96
Source dataset
uspto-grants-2003_09
Patent number
US06617321B2

Reaction notes

Loading…