Formic Acid → HCID 178423993, compound

A solution of 3-methyl-1,2-diaminobenzene (5.00 g, 40.9 mmol) in formic acid (25 mL) was heated at 105° C. for 2 h. The reaction mixture was allowed to cool and then concentrated ammonium hydroxide (50 mL) was added dropwise. The mixture was extracted with dichloromethane (2×100 mL). The extracts were washed with brine, dried (Na2SO4), treated with charcoal, filtered, and evaporated to dryness. The residue was triturated with cold ether, filtered, and washed with cold ether, ether/hexane (1:1), and hexane to give 4-methylbenzimidazole (3.85 g, 71%) as a yellow solid.

1. temperatureto cool
2. extractionThe mixture was extracted with dichloromethane (2×100 mL)
3. washThe extracts were washed with brine
4. dry with materialdried (Na2SO4)
5. additiontreated with charcoal
6. filtrationfiltered
7. customevaporated to dryness
8. customThe residue was triturated with cold ether
9. filtrationfiltered
10. washwashed with cold ether, ether/hexane (1:1), and hexane

ORD record

ord-6d23c67fe655414b8679e54819e56a56

Source dataset

uspto-grants-2001_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06331640B1