Tetrahydrofuran → HCID 86660347、化合物

温度

0 °C

The tetraacid chloride from Step I and dry tetrahydrofuran (50 mL), were mixed under an inert atmosphere and the mixture was cooled to 0° C. for at least 30 min. Dimethyl 5-aminoisophthalate (Aldrich, 2.65 g, 12.7 mmol) is then added as a solution in dry N,N-dimethylformamide (15 mL) in slowly, dropwise to the flask containing the tetraacid chloride chloride. Two successive rinses with tetrahydrofuran (10 mL) were done to quantitatively transfer all of the amine to the acid chloride flask. Triethylamine (2.6 mL, 18.7 mmol) was then added and the reaction is then allowed to slowly warm to room temperature and stir overnight. After removing the tetrahydrofuran by rotary evaporation, the crude residue is then dissolved in 140 mL of diethyl ether, and is washed with deionized water (40 mL), saturated sodium bicarbonate (40 mL), 5% citric acid (40 L), and brine (40 mL). The diethyl ether layer is then dried over sodium sulfate, filtered through glass wool, the solvent removed by rotary evaporation, and dried in vacuo to give crude tetramethyl bis isophthalate (5.61 g) as a viscous, yellow syrup. The diester thus obtained is used in the next step without further purification.

1. temperatureto slowly warm to room temperature
2. customAfter removing the tetrahydrofuran
3. customby rotary evaporation
4. dissolutionthe crude residue is then dissolved in 140 mL of diethyl ether
5. washis washed with deionized water (40 mL), saturated sodium bicarbonate (40 mL), 5% citric acid (40 L), and brine (40 mL)
6. dry with materialThe diethyl ether layer is then dried over sodium sulfate
7. filtrationfiltered through glass wool
8. customthe solvent removed by rotary evaporation
9. customdried in vacuo

ORDレコード

ord-af8ea8a7b9784bb38e04706cf88b628a

出典データセット

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08703988B2