Hydrochloric Acid → HCID 15274145, compound

Nitrogen was introduced into a flask (250 ml), and 10 ml of anhydrous diethyl ether was added, and 15 g of magnesium was added, and stirred. Hexyl bromide (0.61 mole) of 100 g mixed with 50 ml of diethylether was poured into a dropping funnel, and the mixture therein was slowly added into the flask over 1 hour. The reaction was carried out at 45° C. for 3 hours. The reaction product, Grignard, was poured into a dropping funnel. To the reactant was slowly added a mixture of 42 g of 1,4-dichlorobenzene (0.29 mol), 0.3 g of NiCl2 and 80 ml of diethylether, and the reaction was carried out at room temperature for 24 hours to obtain solid reaction product. 6 N HCl was slowly added so as to neutralize the solid reaction product, the product was extracted with diethyl ether and dried with anhydrous MgSO4, and the reaction product was separated by vacuum distillation (122° C./0.1 mmHg). The structure analysis of the compound was confirmed by 1H-NMR, which was shown in FIG. 3.

1. additionwas added
2. additionwas poured into a dropping funnel
3. additionthe mixture therein was slowly added into the flask over 1 hour
4. additionThe reaction product, Grignard, was poured into a dropping funnel
5. additionTo the reactant was slowly added
6. waitthe reaction was carried out at room temperature for 24 hours
7. customto obtain
8. customsolid reaction product
9. customthe solid reaction product
10. extractionthe product was extracted with diethyl ether
11. dry with materialdried with anhydrous MgSO4
12. customthe reaction product was separated by vacuum distillation (122° C./0.1 mmHg)

ORD record

ord-cb3ea11d733f4c7ea312225bb66b756f

Source dataset

uspto-grants-2000_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06124046