1-Bromo-3-methylbutan-2-one → HCID 57666787、化合物
反応式
[N+:1]([C:4]1[CH:12]=[C:11]([C:13]([F:16])([F:15])[F:14])[CH:10]=[CH:9][C:5]=1[C:6]([NH2:8])=[S:7])([O-:3])=[O:2].Br[CH2:18][C:19](=O)[CH:20]([CH3:22])[CH3:21]>O1CCOCC1>[CH:20]([C:19]1[N:8]=[C:6]([C:5]2[CH:9]=[CH:10][C:11]([C:13]([F:16])([F:14])[F:15])=[CH:12][C:4]=2[N+:1]([O-:3])=[O:2])[S:7][CH:18]=1)([CH3:22])[CH3:21]参加物
4
反応条件
- 温度
- 100 °C
実験手順
2-Nitro-4-trifluoromethyl-thiobenzamide (55), (100 mg, 0.4 mmol) was dissolved in dioxan (4 ml) in a 10 ml test tube and to this solution was added 1-bromo-3-methyl-butan-2-one (52) (72.6 mg, 0.44 mmol). A stirrbar was added and the tube was sealed and heated to 100° C. over night. After cooling to ambient temperature, the vessel was de-capped, the solvent removed in vacuo and the residue partitioned between DCM and 10% aqueous NaHCO3 solution. The organic phase was separated and washed with additional 10% aqueous NaHCO3 solution and brine. The organic phase was filtered through a hydrophobic frit and the solvent removed in vacuo which gave the target compound (120 mg, 90%). LC/MS: (Method I): tR=2.26 min, >90%, m/z (ESI)=317 (MH+).