Ethanol → HCID 86653606, compound

HRID 1918260Notes

Reaction equation

HRID 1918260 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].[CH2:30]([OH:32])[CH3:31].C([O:37]C)(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:30]([O-:37])(=[O:32])[CH3:31]

Participants

5

Reactant 3

HCID 702EthanolHCID 15413tert-Butyl methyl etherHCID 5329102Sunitinib

Product 1

HCID 86653606HCID 86653606, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
50 °C

Procedure

Sunitinib base (3 g) was dissolved in acetic acid (6 ml) and absolute ethanol (6 ml) by stirring for 10 min at 20° C. and the solution was heated to 50° C. Then methyl tert-butyl ether (60 ml) was added within 30 min with stirring, the mixture was cooled to −10° C. After 16 h at −10° C. the solid was filtered, washed with 2×20 ml of MTBE, dried on filter for one hour obtaining a red solid.

Workup

  1. temperaturethe mixture was cooled to −10° C
  2. filtrationAfter 16 h at −10° C. the solid was filtered
  3. washwashed with 2×20 ml of MTBE
  4. customdried
  5. filtrationon filter for one hour
  6. customobtaining a red solid

Sources & evidence

ORD record
ord-cf41012f8c01460f96548df0d3a0e70a
Source dataset
uspto-grants-2013_12
Patent number
US08618309B2

Reaction notes

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