反応 #468879

反応方程式

hexadecanol

N-carbamylmaleimide

H2O

→

hexadecyl maleurate

収率 98.0%

溶媒

p-dioxane

反応条件

後処理

1. 1
   温度was heated to reflux
2. 2
   ろ過The resulting solid was filtered
3. 3
   洗浄washed with additional H2O
4. 4
   その他dried

実験手順

A mixture of 49 g of hexadecanol (0.202 moles), 28 g of N-carbamylmaleimide (0.2 moles) and 270 mg of zinc chloride (0.002 moles) in 300 mL of p-dioxane was heated to reflux. After 24 hours, the mixture was cooled to room temperature and 200 mL of H2O was added. The resulting solid was filtered, washed with additional H2O and dried to afford 75 g (97% yield) of hexadecyl maleurate. M.P.: 106°-09° C. (dec.); 1H NMR (CDCl3): δ10.5 (br s, 1H), 8.2 (br s, 1H), 6.3 (m, 2H), 5.4 (br s, 1H), 4.2 (t, 2H), 1.6 (m, 2 H), 1.2 (m, 26H), 0.9 (t, 3H); HPLC (80% CH3CN/H2O, C18): Rt=6.9 minutes.

出典