反応 #70197

反応方程式

NH4Cl

iodomethane

aldehyde

2-Iodo-5-isopropoxy-4-methoxybenzaldehyde

→

title compound 6

収率 100.1%

1-(2-Iodo-5-isopropoxy-4-methoxyphenyl)ethanol

収率 100.1%

溶媒

Et2O

Et2O

Et2O

Et2O

反応条件

後処理

1. 1
   workup.ADDITIONthen treated
2. 2
   温度to warm to 18° C
3. 3
   workup.STIRRINGStirring
4. 4
   洗浄The separated organic phase was washed with H2O (1×5 mL)
5. 5
   乾燥then dried (MgSO4)
6. 6
   ろ過filtered
7. 7
   濃縮concentrated under reduced pressure

実験手順

A mixture of Mg turnings (195 mg, 8.02 g·atom) in dry Et2O (3.0 mL) was stirred at 0° C. under a nitrogen atmosphere then treated, dropwise, with a solution of iodomethane (0.58 mL, 9.31 mmol) in dry Et2O (7.5 mL). After 0.5 h a solution of aldehyde 5 (1.00 g, 3.12 mmol) in dry Et2O (7.5 mL) was added, dropwise, and the ensuing mixture then allowed to warm to 18° C. Stirring was continued at this temperature for a further 1 h then the reaction mixture was treated with NH4Cl (5 mL of a 20% w/v aqueous solution) and Et2O (10 mL). The separated organic phase was washed with H2O (1×5 mL) then dried (MgSO4), filtered and concentrated under reduced pressure to afford the title compound 6 (1.05 g, quant.) as a pale-yellow oil.

出典