Hydrochloric Acid → HCID 20042126, compound

HRID 1762085Notes

Reaction equation

HRID 1762085 reaction equation
[NH2:1][C:2]1[C:3]([N+:15]([O-])=O)=[CH:4][C:5]2[NH:10][C:9](=[O:11])[O:8][C:7]([CH3:13])([CH3:12])[C:6]=2[CH:14]=1.[H][H].[ClH:20]>CO.[Pd]>[ClH:20].[ClH:20].[NH2:1][C:2]1[C:3]([NH2:15])=[CH:4][C:5]2[NH:10][C:9](=[O:11])[O:8][C:7]([CH3:12])([CH3:13])[C:6]=2[CH:14]=1

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 20042218HCID 20042218, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 20042126HCID 20042126, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

35.6 g (0.15 mol) of 6-amino-4,4-dimethyl-7-nitro-4H-3,1-benzoxazin-2-one are dissolved in 500 ml of methanol and 60 ml of 7.5 N methanolic hydrochloric acid, 3.5 g of 10% Palladium/charcoal are added and the resulting mixture is hydrogenated for 45 minutes in an autoclave at ambient temperature under 5 bar of hydrogen pressure. The catalyst is then removed by suction filtering and the filtrate is diluted to 2 liters with ether. The precipitate is suction filtered, washed with ether and dried.

Workup

  1. customThe catalyst is then removed by suction
  2. filtrationfiltering
  3. additionthe filtrate is diluted to 2 liters with ether
  4. filtrationfiltered
  5. washwashed with ether
  6. customdried

Sources & evidence

ORD record
ord-737790275de640258bd3dc936e639ea0
Source dataset
uspto-grants-1989_05
Patent number
US04831027

Reaction notes

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