Hydroxylamine → HCID 23339651, compound

HRID 1112431Notes

Reaction equation

HRID 1112431 reaction equation
[C:1]1([NH:11][C:12]([CH2:14][C:15]([O:17]CC)=O)=[O:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[NH2:20][OH:21].Cl.NO.[Na]>CO>[C:1]1([NH:11][C:12]([CH2:14][C:15]([NH:20][OH:21])=[O:17])=[O:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

Participants

6

Reactant 4

HCID 787HydroxylamineHCID 443297Hydroxyamine hydrochlorideHCID 5360545SodiumHCID 12547460Ethyl alpha-naphthylcarbamoylacetate

Product 1

HCID 23339651HCID 23339651, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

19.3 g (0.075 mol) of ethyl α-naphthylcarbamoylacetate are treated with a solution of hydroxylamine, prepared from 5.6 g (0.08 mol) of hydroxylamine hydrochloride and 3.68 g of sodium in 250 ml of methanol. After leaving the reactants in contact for 5 hours, the mixture is evaporated to dryness in vacuo, the residue is taken up in 400 ml of cold water, the solution is filtered over charcoal, and the product is precipitated cold with 3N HCl, filtered off and washed with water. CRL 40,518 is obtained by recrystallisation from ethanol.

Workup

  1. customAfter leaving the reactants in contact for 5 hours
  2. customthe mixture is evaporated to dryness in vacuo
  3. filtrationthe solution is filtered over charcoal
  4. customthe product is precipitated cold with 3N HCl
  5. filtrationfiltered off
  6. washwashed with water
  7. customCRL 40,518 is obtained by recrystallisation from ethanol

Sources & evidence

ORD record
ord-bbd26462549444f0be0ea548b529d91c
Source dataset
uspto-grants-1978_10
Patent number
US04122186

Reaction notes

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