癸腈

反应条件: temp:105.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a stirred vessel fitted with reflux condenser and dropping funnel, 317 g of o-xylene were initially charged, 198.96 g of solid potassium methoxide were added and the mixture was heated at reflux. A mixture of 170 g of decanonitrile and 133.9 g of ethyl acetate was then added via the dropping funnel over a period of 10 min. After the addition had ended, stirring was continued for 4 h, and the mixture was then cooled to 105° C. 372 g of water were then added, and the mixture was adjusted to pH 4.3 by addition of about 470 g of 20% strength hydrochloric acid. The temperature was set to 65° C., and the (lower) aqueous phase was removed. The organic phase was washed with another 186 g of water. After removal of the aqueous phase, the organic phase was concentrated to about half of its original volume to remove the water. This gave 211.7 g of a light-yellow solution having a content of product of value of 66.8% a/a (GC), which solution can be reacted further as such. For purification, the compound was distilled under high vacuum, with the product passing over at 106 to 121° C./1 mbar. In a stirred vessel fitted with reflux condenser the mixture was heated at reflux was then added via the dropping funnel over a period of 10 min After the addition was set to 65° C. the (lower) aqueous phase was removed The organic phase was washed with another 186 g of water After removal of the aqueous phase the organic phase was concentrated to about half of its original volume to remove the water can be reacted further as such For purification the compound was distilled under high vacuum, with the product passing over at 106 to 121° C./1 mbar

反应条件: temp:105.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a stirred vessel fitted with reflux condenser and dropping funnel, 199.96 g of solid potassium methoxide were initially charged, and 318 g of o-xylene were added. 15 g of ethanol were added, and the suspension was heated to reflux. A mixture of 170 g of decanonitrile and 180.8 g of ethyl methoxy acetate was then added via the dropping funnel over a period of 10 min. After the addition had ended, stirring was continued for 6 h, and the mixture was then cooled to 105° C. 373 g of water were then added, and the mixture was adjusted to pH 4 by addition of about 388 g of 20% strength hydrochloric acid. The temperature was set to 70° C., and the (lower) aqueous phase was removed. The organic phase was washed with another 186 g of water. After removal of the aqueous phase, the organic phase was concentrated to half of its original volume in order to remove the water. This gave 235.5 g of a pale yellow solution having a content of product of value of 62% a/a (GC), which can be reacted further as such. For purification, the compound was distilled under high vacuum, with the product passing over at 120 to 134° C./1 mbar. In a stirred vessel fitted with reflux condenser the suspension was heated to reflux was then added via the dropping funnel over a period of 10 min After the addition was set to 70° C. the (lower) aqueous phase was removed The organic phase was washed with another 186 g of water After removal of the aqueous phase the organic phase was concentrated to half of its original volume in order to remove the water can be reacted further as such For purification the compound was distilled under high vacuum, with the product passing over at 120 to 134° C./1 mbar

反应条件: temp:105.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a stirred vessel fitted with reflux condenser and dropping funnel, 317 g of o-xylene were initially charged, 198.96 g of solid potassium methoxide were added and the mixture was heated at reflux. A mixture of 170 g of decanonitrile and 133.9 g of ethyl acetate was then added via the dropping funnel over a period of 10 min. After the addition had ended, stirring was continued for 4 h, and the mixture was then cooled to 105° C. 372 g of water were then added, and the mixture was adjusted to pH 4.3 by addition of about 470 g of 20% strength hydrochloric acid. The temperature was set to 65° C., and the (lower) aqueous phase was removed. The organic phase was washed with another 186 g of water. After removal of the aqueous phase, the organic phase was concentrated to about half of its original volume to remove the water. This gave 211.7 g of a light-yellow solution having a content of product of value of 66.8% a/a (GC), which solution can be reacted further as such. For purification, the compound was distilled under high vacuum, with the product passing over at 106 to 121° C./1 mbar. In a stirred vessel fitted with reflux condenser the mixture was heated at reflux was then added via the dropping funnel over a period of 10 min After the addition was set to 65° C. the (lower) aqueous phase was removed The organic phase was washed with another 186 g of water After removal of the aqueous phase the organic phase was concentrated to about half of its original volume to remove the water can be reacted further as such For purification the compound was distilled under high vacuum, with the product passing over at 106 to 121° C./1 mbar

反应条件: temp:105.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: In a stirred vessel fitted with reflux condenser and dropping funnel, 199.96 g of solid potassium methoxide were initially charged, and 318 g of o-xylene were added. 15 g of ethanol were added, and the suspension was heated to reflux. A mixture of 170 g of decanonitrile and 180.8 g of ethyl methoxy acetate was then added via the dropping funnel over a period of 10 min. After the addition had ended, stirring was continued for 6 h, and the mixture was then cooled to 105° C. 373 g of water were then added, and the mixture was adjusted to pH 4 by addition of about 388 g of 20% strength hydrochloric acid. The temperature was set to 70° C., and the (lower) aqueous phase was removed. The organic phase was washed with another 186 g of water. After removal of the aqueous phase, the organic phase was concentrated to half of its original volume in order to remove the water. This gave 235.5 g of a pale yellow solution having a content of product of value of 62% a/a (GC), which can be reacted further as such. For purification, the compound was distilled under high vacuum, with the product passing over at 120 to 134° C./1 mbar. In a stirred vessel fitted with reflux condenser the suspension was heated to reflux was then added via the dropping funnel over a period of 10 min After the addition was set to 70° C. the (lower) aqueous phase was removed The organic phase was washed with another 186 g of water After removal of the aqueous phase the organic phase was concentrated to half of its original volume in order to remove the water can be reacted further as such For purification the compound was distilled under high vacuum, with the product passing over at 120 to 134° C./1 mbar