Epichlorohydrin → Oxirane, 2-[[(6-methylheptyl)oxy]methyl]-

온도

130 °C

A reactor of the kind described in Example 8 is charged with 130.23 g (1.0 mol) of isooctanol (mixture of isomers), 5.57 g (0.02 mol) of powdered tin dibromide and 5.28 g (0.02 mol) of 18-crown-6 (crown ether) and the charge is heated to 130° C. Then, with efficient stirring, 86.26 ml (1.1 mol) of epichlorohydrin are added over 30 minutes. The reaction is allowed to continue for 12 hours, during which time the temperature rises to about 135° C. The reaction mixture is cooled to 55° C. and then, at this temperature, 88 g (1.1 mol) of a 50% solution of sodium hydroxide are added dropwise with efficient stirring over 30 minutes. After stirring for 2.5 hours at 55°-60° C. and cooling to room temperature, the suspension is filtered and the filtrate is washed with ethyl acetate. The phases are separated, and the aqueous phase is extracted once with 100 ml of ethyl acetate. The combined organic phases are washed with as small an amount of 10% KH2PO4 solution as possible and then with water until neutral, dried over magnesium sulfate and filtered. The filtrate is freed from solvent on a rotary evaporator under vacuum (bath temperature 50° C.). Yield: 181.8 g (98% of theory) of yellowish isooctanol glycidyl ether (mixture of isomers) for which the following analytical values are obtained: epoxy value: 3.69 eq/kg (69% of theory); total chlorine content: 3.31%; hydrolysable chlorine content: 750 ppm.

1. customA reactor of the kind described in Example 8
2. customrises to about 135° C
3. temperatureThe reaction mixture is cooled to 55° C.
4. stirringAfter stirring for 2.5 hours at 55°-60° C.
5. temperaturecooling to room temperature
6. filtrationthe suspension is filtered
7. washthe filtrate is washed with ethyl acetate
8. customThe phases are separated
9. extractionthe aqueous phase is extracted once with 100 ml of ethyl acetate
10. washThe combined organic phases are washed with as small an amount of 10% KH2PO4 solution as possible and then with water until neutral,
11. dry with materialdried over magnesium sulfate
12. filtrationfiltered
13. customThe filtrate is freed from solvent on a rotary evaporator under vacuum (bath temperature 50° C.)

ORD 기록

ord-95389b7f4fc7473f977f16706fc4c031

출처 데이터셋

uspto-grants-1992_11

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05162547