Acetone → HCID 131734373, compound

HRID 1507463Notes

Reaction equation

[CH3:1][CH2:2][CH2:3][S:4]([NH:7][C:8]1[CH:9]=[CH:10][C:11]([F:33])=[C:12]([C:15]([C:17]2[C:21]3[CH:22]=[C:23]([C:26]4[CH:27]=[CH:28][C:29]([Cl:32])=[CH:30][CH:31]=4)[CH:24]=[N:25][C:20]=3[NH:19][CH:18]=2)=[O:16])[C:13]=1[F:14])(=[O:6])=[O:5].CC(C)=O.[OH:38][CH2:39][CH2:40][N+:41]([CH3:44])([CH3:43])[CH3:42]>C(O)(C)C>[CH3:1][CH2:2][CH2:3][S:4]([NH:7][C:8]1[CH:9]=[CH:10][C:11]([F:33])=[C:12]([C:15]([C:17]2[C:21]3[CH:22]=[C:23]([C:26]4[CH:27]=[CH:28][C:29]([Cl:32])=[CH:30][CH:31]=4)[CH:24]=[N:25][C:20]=3[NH:19][CH:18]=2)=[O:16])[C:13]=1[F:14])(=[O:6])=[O:5].[OH:38][CH2:39][CH2:40][N+:41]([CH3:44])([CH3:43])[CH3:42]

Participants

Conditions

Temperature: 35 °C

Procedure

To a stirred suspension of 5 g Vemurafenib base and 50 ml acetone (T=30-35° C.), 3.0 ml choline (45% in methanol) was added. The obtained solution was stirred for 5 min at 35° C. and then cooled to RT. After evaporation of the solvent, a solid was obtained. 15 ml isopropanol was added, the suspension was placed in an ultrasonic bath (suspension, no solution was formed) and then stored in the refrigerator for 1 days. The precipitate was filtered off, washed with 5 ml isopropanol and dried at RT O/N. 2.07 g (yield: 80.5%).

Workup

additionwas added
temperaturecooled to RT
customAfter evaporation of the solvent
customa solid was obtained
customthe suspension was placed in an ultrasonic bath
custom(suspension, no solution was formed) and
waitthen stored in the refrigerator for 1 days
filtrationThe precipitate was filtered off
washwashed with 5 ml isopropanol
customdried at RT O/N

Sources & evidence

ORD record: ord-66db14130b6b4087be1f9205bf184709
Source dataset: uspto-grants-2015_12
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US09221815B2

Reaction notes

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