Methane → HCID 13055794, compound

HRID 615427Notes

Reaction equation

HRID 615427 reaction equation
[Cl:1][C:2]1[C:11]2[N:10]([CH3:12])[CH2:9][CH:8]([CH3:13])[N:7]3[CH:14]=[C:15]([C:18]([O:20]CC)=[O:19])[C:16](=[O:17])[C:5]([C:6]=23)=[CH:4][CH:3]=1.C>[OH-].[Na+]>[Cl:1][C:2]1[C:11]2[N:10]([CH3:12])[CH2:9][CH:8]([CH3:13])[N:7]3[CH:14]=[C:15]([C:18]([OH:20])=[O:19])[C:16](=[O:17])[C:5]([C:6]=23)=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 297MethaneHCID 13055793HCID 13055793, compound

Product 1

HCID 13055794HCID 13055794, compound

Reagents, catalysts & solvents 1

HCID 14798Sodium HydroxideSolvent

Procedure

A mixture of 13.8 g of ethyl 10-chloro-2,3-dihydro-1,3-dimethyl-7-oxo-1H, 7H-pyrido[1,2,3-de]quinoxaline-6-carboxylate and 600 ml of three percent sodium hydroxide solution is heated on a steam bath for five hours. The solution is treated with decolorizing charcoal, filtered and neutralized to pH 7 with acetic acid. The product is separated by filtration, washed with water and recrystallized from N,N-dimethylformamide to provide yellow crystals of 10-chloro-2,3-dihydro-1,3-dimethyl-7-oxo-1H,7H-pyrido[1,2,3-de]quinoxaline-6-carboxylic acid, m.p. 243°-245° C. Analysis: Calculated for C14H13ClN2O3 : %C, 57.5; %H, 4.5; %N, 9.6. Found %C, 58.0; %H, 4.3; %N, 9.7.

Workup

  1. temperatureis heated on a steam bath for five hours
  2. filtrationfiltered
  3. customThe product is separated by filtration
  4. washwashed with water
  5. customrecrystallized from N,N-dimethylformamide

Sources & evidence

ORD record
ord-9c3857c73c444d668d015b490997c809
Source dataset
uspto-grants-1985_02
Patent number
US04499270

Reaction notes

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