Boron tribromide → Ethyl 3-hydroxy-4-methylphenylacetate
反応式
C[O:2][C:3]1[CH:4]=[C:5]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH:6]=[CH:7][C:8]=1[CH3:9].B(Br)(Br)Br>C(Cl)Cl>[OH:2][C:3]1[CH:4]=[C:5]([CH2:10][C:11]([O:13][CH2:14][CH3:15])=[O:12])[CH:6]=[CH:7][C:8]=1[CH3:9]参加物
4
反応条件
- 温度
- -78 °C
実験手順
step 3—To a solution of 4c (2.2 g; 8.0 mmol) and 250 mL CH2Cl2 cooled to −78° C. was added dropwise via syringe BBr3 (9.8 mL; 0.104 mol). After 1 h at −78° C. the reaction was stirred for 4 h in an ice-water bath. The reaction mixture was recooled to −78° C. and the reaction quenched aqueous NaHCO3 then warmed to rt and the organic phase washed with water, saturated NaHCO3 and brine. The organic phase was dried (MgSO4) and the solvent evaporated to afford 1.4 g of ethyl 3-hydroxy-4-methylphenylacetate (6).
後処理
- customwas recooled to −78° C.
- customthe reaction quenched aqueous NaHCO3
- temperaturethen warmed to rt
- washthe organic phase washed with water, saturated NaHCO3 and brine
- dry with materialThe organic phase was dried (MgSO4)
- customthe solvent evaporated
出典と根拠
- ORDレコード
- ord-d262bb240e7847a582518adfab8ed679
- 出典データセット
- uspto-grants-2012_12
- 特許番号
- US08329755B2
反応ノート
読み込み中…