Sodium Hydroxide → HCID 19913960, compound

HRID 1090767Notes

Reaction equation

HRID 1090767 reaction equation
[N:1]([C:3]1[C:12]2[C:7](=[CH:8][C:9]([C:13]([O:15][CH3:16])=[O:14])=[CH:10][CH:11]=2)[CH:6]=[CH:5][C:4]=1[OH:17])=O.[S:18]([O-:21])([OH:20])=[O:19].[Na+].[OH-].[Na+]>O>[NH2:1][C:3]1[C:12]2[C:7](=[CH:8][C:9]([C:13]([O:15][CH3:16])=[O:14])=[CH:10][CH:11]=2)[C:6]([S:18]([OH:21])(=[O:20])=[O:19])=[CH:5][C:4]=1[OH:17]

Participants

5

Reactant 3

HCID 14798Sodium HydroxideHCID 19913958HCID 19913958, compoundHCID 23665763Sodium Bisulfite

Product 1

HCID 19913960HCID 19913960, compoundYield 64%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
40 °C

Procedure

92.4 g (0.4 mol) of crude 1-nitroso-6-methoxycarbonyl-β-naphthol were added at room temperature to a solution of 360 g (1.11 mol) of 40%-strength aqueous sodium hydrogen sulfite and 4.4 g (0.11 mol) or sodium hydroxide in 1610 ml of water. The suspension was heated for 24 h at 40° C. and then 2.4 g; (2.6% of the amount taken) of residue were separated off. The clear solution was then acidified at 25° C. with 142 g (1.39 mol) of 36%-strength sulfuric acid and the product was crystallized out for 48 hours at room temperature. After filtration by suction and drying, 76.0 g (64%) of product is obtained.

Workup

  1. customwere separated off
  2. customwas then acidified at 25° C. with 142 g (1.39 mol) of 36%-strength sulfuric acid
  3. customthe product was crystallized out for 48 hours at room temperature
  4. filtrationAfter filtration by suction
  5. customdrying

Sources & evidence

ORD record
ord-dcf53210ba324c8894e2331a18e58e12
Source dataset
uspto-grants-1992_01
Patent number
US05082932

Reaction notes

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