Acetic Acid → HCID 86653606, compound

HRID 1918258Notes

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:30]([OH:33])(=[O:32])[CH3:31]>C(O)CCC>[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-:33])(=[O:32])[CH3:31]

Participants

Conditions

Temperature: 20 °C

Procedure

Sunitinib base (1.5 g) was suspended in n-butanol (7.5 ml) and acetic acid (2.3 ml) was added in one portion with stirring at 20° C. Adding of acetic acid facilitated complete dissolution of sunitinib base within 2 minutes. The solution was stirred for 60 minutes during which orange precipitate was formed. The precipitate was recovered by filtration, washed with t-butyl methyl ether (50 ml) and dried on air for 12 h at 20° C. (Yield 1.074 g).

Workup

stirringThe solution was stirred for 60 minutes during which orange precipitate
customwas formed
filtrationThe precipitate was recovered by filtration
washwashed with t-butyl methyl ether (50 ml)
customdried on air for 12 h at 20° C. (Yield 1.074 g)

Sources & evidence

ORD record: ord-efb85e4745bf4c5b8db9dea7737b318c
Source dataset: uspto-grants-2013_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08618309B2

Reaction notes

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