Chloroform → HCID 178463596, compound

The product of step (i) (11.85 g) was dissolved in 2N NaOH (270 ml) and 10N NaOH (27 ml) and heated to 65° C. Within 1.25 hours 50% Ni—Al alloy (518 mmoles of Ni and 1125 mmoles of Al) (60.8 g) was added under vigorous string at 65-70° C. After a further 0.75 hr at the same temperature the reaction mixture was cooled to room temperature and treated with chloroform (400 ml). The nickel was filtered off and washed with 350 ml of chloroform and 150 ml of water. The filtrate was separated and the chloroform layer evaporated to dryness. The residue (19.64 g) was dissolved in acetone (100 ml), treated with 2 portions of charcoal (0.15 g) filtered, and evaporated. The residue was treated with diethylether (100 ml) and crystals collected (6.10 g), mp 80-96° C. A second crop gave 1.25 g. A recrystallized sample from diisopropylether had mp 103-105° C.

1. filtrationThe nickel was filtered off
2. washwashed with 350 ml of chloroform and 150 ml of water
3. customThe filtrate was separated
4. customthe chloroform layer evaporated to dryness
5. dissolutionThe residue (19.64 g) was dissolved in acetone (100 ml)
6. additiontreated with 2 portions of charcoal (0.15 g)
7. filtrationfiltered
8. customevaporated
9. additionThe residue was treated with diethylether (100 ml) and crystals
10. customcollected (6.10 g), mp 80-96° C
11. customA second crop gave 1.25 g

ORD record

ord-f42b3219b1e64eb098fd3a30e3d32688

Source dataset

uspto-grants-2001_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06319928B1