Trifluoroacetic acid → HCID 14556369, compound
Reaction equation
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([C:11](=O)[CH:12]([CH3:15])[CH2:13][Br:14])=[CH:10][C:5]=2[O:4][C:3]1=[O:17].FC(F)(F)C(O)=O.C([SiH](CC)CC)C>>[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][CH:12]([CH3:15])[CH2:13][Br:14])=[CH:10][C:5]=2[O:4][C:3]1=[O:17]Participants
4
Procedure
0.03 mole of 3-methyl-6-(3-bromo-2-methylpropionyl)benzoxazolinone is dissolved in 0.3 mole of trifluoroacetic acid in a 150-cm3 flask. 0.066 mole of triethylsilane is added dropwise and with cooling. Stirring is continued for 24 hours at room temperature. The reaction mixture is poured into 5 volumes of ice-cold water. The precipitate obtained is drained, washed with water until the washing liquors are neutral, dried and recrystallized in cyclohexane.
Workup
- temperaturewith cooling
- additionThe reaction mixture is poured into 5 volumes of ice-cold water
- customThe precipitate obtained
- washwashed with water until the washing liquors
- customdried
- customrecrystallized in cyclohexane
Sources & evidence
- ORD record
- ord-fa92d19c905a48ac8e5a48c680f4849c
- Source dataset
- uspto-grants-1990_10
- Patent number
- US04960778
Reaction notes
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