反応 #741808

反応方程式

diethyl 2-(3-methoxy-5-(methylthio)-4-propoxyphenyl)-2,5-dicyano-5-(3,4,5-trimethoxyphenyl)-1,6-hexanedioate

potassium hydroxide

→

5-(3,4,5-trimethoxyphenyl)-1,6-hexanedinitrile

収率 66.0%

溶媒

ethanol

反応条件

後処理

1. 1
   ろ過filtered
2. 2
   濃縮the filtrate concentrated
3. 3
   workup.ADDITIONMethanol (300 ml) was added to the residue
4. 4
   ろ過The reaction was filtered
5. 5
   その他the precipitate dried

実験手順

To a solution of diethyl 2-(3-methoxy-5-(methylthio)-4-propoxyphenyl)-2,5-dicyano-5-(3,4,5-trimethoxyphenyl)-1,6-hexanedioate (12.0 g, 0.019 mol) in ethanol (250 ml) was added potassium hydroxide (4.4 g, 0.079 mol). The reaction was heated to 95° C. for 20 minutes, then filtered, and the filtrate concentrated. Methanol (300 ml) was added to the residue, and the solution was stirred at room temperature overnight. The reaction was filtered and the precipitate dried to yield 2-(3-methoxy-5-methylthio)-4-propoxyphenyl)-5-(3,4,5-trimethoxyphenyl)-1,6-hexanedinitrile in a 66% yield. (m.p. 131°-132.5° C.). NMR (CDCl3): δ 1.04 (t, 3H, term CH3), 1.80 (m, 2H, OCH2CH2CH3), 2.18 (m, 2H, CH2 from ##STR30## 2.44 (m+s, SCH3 --CH2 from ##STR31## 3.90 (m, 14H, --OCH3 +OCH2CH2CH3), 6.64+6.72 (s, 2H, ArH), 6.71, 6.77, 6.81, 6.83 (d,d, 2H, ArH).

出典