Diisopropyl Ether → HCID 86653606, compound

HRID 1918259Notes

Reaction equation

HRID 1918259 reaction equation
[CH3:1][CH2:2][N:3]([CH2:6][CH2:7][NH:8][C:9]([C:11]1[C:15]([CH3:16])=[C:14](/[CH:17]=[C:18]2/[C:19]3[CH:24]=[C:23]([F:25])[CH:22]=[CH:21][C:20]=3[NH:26][C:27]/2=[O:28])[NH:13][C:12]=1[CH3:29])=[O:10])[CH2:4][CH3:5].C([O:33][CH:34]([CH3:36])C)(C)C>C(O)(=O)C>[CH3:1][CH2:2][N:3]([CH2:6][CH2:7][NH:8][C:9]([C:11]1[C:15]([CH3:16])=[C:14](/[CH:17]=[C:18]2/[C:19]3[CH:24]=[C:23]([F:25])[CH:22]=[CH:21][C:20]=3[NH:26][C:27]/2=[O:28])[NH:13][C:12]=1[CH3:29])=[O:10])[CH2:4][CH3:5].[C:34]([O-:10])(=[O:33])[CH3:36]

Participants

4

Conditions

Temperature
20 °C

Procedure

Sunitinib base (1.3 g) was dissolved in acetic acid (10 ml) by stirring for 5 min at 20° C. Then diisopropyl ether (20 min) was added within 30 min with stirring. Then the solution was filtered and t-butyl methyl ether (50 ml) was added to the stirred solution within 5 min. The orange precipitate thus formed was recovered by filtration, washed with t-butyl methyl ether (50 ml) and dried on air for 12 h at 20° C. (Yield 1.425 g).

Workup

  1. stirringwith stirring
  2. filtrationThen the solution was filtered
  3. additiont-butyl methyl ether (50 ml) was added to the stirred solution within 5 min
  4. customThe orange precipitate thus formed
  5. filtrationwas recovered by filtration
  6. washwashed with t-butyl methyl ether (50 ml)
  7. customdried on air for 12 h at 20° C. (Yield 1.425 g)

Sources & evidence

ORD record
ord-f0c9376683694da9812f2673f2ac66e6
Source dataset
uspto-grants-2013_12
Patent number
US08618309B2

Reaction notes

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