反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
Into a 25 mL flask was added 527 mg (1.16 mmol) of 2-[5-(4-bromophenoxymethyl)-1 (2,6-dichlorophenyl)-1H-pyrazol-3-yl]-propan-2-ol, 278 μL (1.74 mmol) Triethylsilane and 2 mL of Trifluoroacetic acid. After 1 h the crude reaction was concentrated in vacuo, washed into a separatory funnel with ethyl acetate and NaHCO3. The ethyl acetate was separated, washed with brine, dried (Na2SO4), and concentrated in vacuo to afford 5-(4-bromophenoxymethyl)-1-(2,6-dichlorophenyl)-3-isopropyl-1H-pyrazole as an off white solid (450 mg, 99%); 1H NMR (400 MHz, CDCl3): δ 7.42 (m, 1H), 7.41 (s, 1H), 7.33 (m, 1H), 7.31 (d J=9.1 Hz 2H), 6.67 (d J=9.1 Hz 2H), 6.36 (s, 1H), 4.82 (s, 2H), 4.43 (q, J=7.07 Hz 2H), 1.58 (s, 6H), MS (ES): 439 [M+H]+.
WORKUP
后处理
- customAfter 1 h the crude reaction
- concentrationwas concentrated in vacuo
- washwashed into a separatory funnel with ethyl acetate and NaHCO3
- customThe ethyl acetate was separated
- washwashed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated in vacuo