Tetrahydrofuran → HCID 136343917, compound

HRID 2357112Notes

Reaction equation

HRID 2357112 reaction equation
[CH2:1]1[CH2:5][O:4][CH2:3][CH2:2]1.[CH3:6][C:7]1[S:11][C:10]2[NH:12][C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=3[N:19]=[C:20]([N:21]3[CH2:26][CH2:25][N:24]([CH3:27])[CH2:23][CH2:22]3)[C:9]=2[CH:8]=1>O>[CH3:6][C:7]1[S:11][C:10]2[NH:12][C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:18]=3[N:19]=[C:20]([N:21]3[CH2:22][CH2:23][N:24]([CH3:27])[CH2:25][CH2:26]3)[C:9]=2[CH:8]=1.[OH2:4].[O:4]1[CH2:5][CH2:1][CH2:2][CH2:3]1

Participants

4

Reactant 2

HCID 8028TetrahydrofuranHCID 135398745Olanzapine

Product 1

HCID 136343917HCID 136343917, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
50 °C

Procedure

A mixture made up of 100 mL of THF, 25 mL of water and 25 g of crude anhydrous olanzapine obtained by following the method described in patent EP0454436B1 is heated for 30 min at 50° C. After cooling first to 20-25° C. for one hour and then to 0° C. over a further hour, the solid is filtered and dried in an air oven at 42° C. to constant weight, yielding 24.9 g (85%) of mixed solvate of olanzapine/water/tetrahydrofuran in the proportion 1:1:1/2.

Workup

  1. customobtained
  2. temperatureAfter cooling first to 20-25° C. for one hour
  3. waitto 0° C. over a further hour
  4. filtrationthe solid is filtered
  5. customdried in an air oven at 42° C. to constant weight

Sources & evidence

ORD record
ord-8801958e6f964547ba0406a5d529cd71
Source dataset
uspto-grants-2010_07
Patent number
US07759484B2

Reaction notes

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