Toluene → HCID 23702061, compound

In a flask equipped with a dropping-funnel and a mechanical stirrer were placed 30 g (0.161 mol) of pure tri-n-propylacetic acid prepared as described above and 75 g of toluene. The mixture was stirred until dissolution after which a hot solution of 6.45 g of sodium hydroxide in 30 g of Methanol was added through the dropping-funnel. To the solution thus obtained was added 1g of CECA WSL black after which the whole was refluxed for 1 hour while being stirred. The black was filtered off and the residual mixture was distilled by adding little-by-little through the dropping-funnel 88 g of toluene to prevent the mixture from forming a mass. Distillation was suspended when the temperature at the head of the column reached 105°C, after which the mixture was cooled to room-temperature The precipitate which formed was centrifuged out and rinsed twice with 20 g of acetone. It was then dried in a rotatory evaporator at 80°C for 2 hours and then at 105°C under atmospheric pressure in a ventilated drying-oven for 4 hours. In this way, 30 g of sodium tri-n-propylacetate were obtained which represents a yield of 89.5%.

1. customIn a flask equipped with a dropping-funnel and a mechanical stirrer
2. customprepared
3. additionwas added through the dropping-funnel
4. customTo the solution thus obtained
5. temperaturewas refluxed for 1 hour
6. filtrationThe black was filtered off
7. distillationthe residual mixture was distilled
8. additionby adding little-by-little through the dropping-funnel 88 g of toluene
9. customfrom forming a mass
10. distillationDistillation
11. customreached 105°C
12. temperatureafter which the mixture was cooled to room-temperature The precipitate which
13. customformed
14. washrinsed twice with 20 g of acetone
15. customIt was then dried in a rotatory evaporator at 80°C for 2 hours

ORD record

ord-ce2e7c46bde44971beeb73fe4470351d

Source dataset

uspto-grants-1976_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03958011