Hydroquinone → Ethyl 3,3-diethoxypropylmethylphosphinate

温度

-10 °C

Into a 100 ml. red flask was introduced 12.5 g. of acrolein, and 15 mg. of hydroquinone and 45 ml. of anhydrous ethyl alcohol were added thereto. The resulting mixture was stirred at -10° C. in a stream of nitrogen and then 13.6 g. of diethyl methylphosphonite was added dropwise thereto over 20 minutes. After stirring further for 30 minutes at the same temperature, the mixture was stirred for 2 hours at 0° C. and subsequently for 4 hours at room temperature, followed by further reaction at 70° C. for 12 hours. After the reaction mixture thus obtained was concentrated by evaporation of the ethanol under reduced pressure, the residue was subjected to distillation under reduced pressure to give a fraction boiling at 85° to 91° C./0.17 mmHg. and thus was obtained 12.2 g. of a light-yellow oil of ethyl, 3,3-diethoxypropylmethylphosphinate.

1. additionred flask was introduced 12.5 g
2. stirringAfter stirring further for 30 minutes at the same temperature
3. stirringthe mixture was stirred for 2 hours at 0° C. and subsequently for 4 hours at room temperature
4. customfollowed by further reaction at 70° C. for 12 hours
5. customAfter the reaction mixture thus obtained
6. concentrationwas concentrated by evaporation of the ethanol under reduced pressure
7. distillationthe residue was subjected to distillation under reduced pressure
8. customto give a fraction boiling at 85° to 91° C./0.17 mmHg
9. customand thus was obtained 12.2 g

ORDレコード

ord-8e778a388e9d4cc090294a9c38df8739

出典データセット

uspto-grants-1981_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04264532