反応 #2329035

反応方程式

Thionyl chloride

4-ethoxybenzyl alcohol

DMF

→

4-Ethoxybenzyl Chloride

溶媒

CH2Cl2

CH2Cl2

反応条件

後処理

1. 1
   workup.ADDITIONUpon addition, reaction
2. 2
   その他Reaction mixture
3. 3
   濃縮was concentrated under reduced pressure
4. 4
   workup.DISSOLUTIONthe residue dissolved in minimal THF
5. 5
   その他precipitated in cold H2O
6. 6
   その他to yield a white precipitate
7. 7
   その他The solid was collected
8. 8
   その他dried
9. 9
   濃縮concentrated
10. 10
    温度by cooling with CO2/acetone

実験手順

Thionyl chloride (10.4 g, 87.7 mmol) was added dropwise to a 0° C. solution of 4-ethoxybenzyl alcohol (11.0 g, 72.4 mmol) in dry CH2Cl2 (150 mL) with a catalytic amount of DMF (1 mL). Upon addition, reaction was allowed to stir for 5-10 minutes, while monitoring through TLC (CH2Cl2) for completion. Reaction mixture was concentrated under reduced pressure and the residue dissolved in minimal THF and then precipitated in cold H2O to yield a white precipitate. The solid was collected, taken up in CH2Cl2, dried and concentrated. The resulting oil was solidified by cooling with CO2/acetone. The compound as a white solid, which decomposes upon melting 11.3 g(92%).

出典