Acetic Acid → HCID 117853300, compound
Reaction equation
[CH3:1][C:2]1[C:10]2[C:9]([O:11][CH2:12][C:13]3[O:17][N:16]=[C:15]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[CH:14]=3)=[N:8][CH:7]=[N:6][C:5]=2[S:4][CH:3]=1.ClCCl.[C:27]([OH:30])(=[O:29])[CH3:28]>>[C:27]([OH:30])(=[O:29])[CH3:28].[CH3:1][C:2]1[C:10]2[C:9]([O:11][CH2:12][C:13]3[O:17][N:16]=[C:15]([C:18]4[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=4)[CH:14]=3)=[N:8][CH:7]=[N:6][C:5]=2[S:4][CH:3]=1Participants
4
Procedure
0.5 mmol of 5-methyl-4-((3-phenyl-isoxazol-5-yl)-methoxy-)-thieno[2,3-d]pyrimidine was added into a 50 ml single-necked round-bottom flask containing 10 ml of dry dichloromethane. 2 ml of acetic acid was added under stirring, and the mixture was stirred for 1-2 hours at 30-40. The mixture was cooled down, crystallized, filtered and dried under vacuum to afford 5-methyl-4-((3-phenyl-isoxazol-5-yl)-methoxy-)-thieno[2,3-d]pyrimidine acetate as a colorless solid in 58% yield.
Workup
- stirringthe mixture was stirred for 1-2 hours at 30-40
- temperatureThe mixture was cooled down
- customcrystallized
- filtrationfiltered
- customdried under vacuum
Sources & evidence
- ORD record
- ord-d9c2c71abb9045cc80015f3e8759c6b9
- Source dataset
- uspto-grants-2016_09
- Patent number
- US09434741B2
Reaction notes
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