Sodium Hydroxide → HCID 18694061, compound

HRID 1870817Notes

Reaction equation

HRID 1870817 reaction equation
[CH3:1][S:2]([NH:5][C:6]([CH2:8][C:9]1[C:10]2[CH2:11][C:12]3[N:17]4[CH:18]=[C:19]([C:21]([O:23]CC)=[O:22])[N:20]=[C:16]4[C:15](=[O:26])[NH:14][C:13]=3[C:27]=2[CH:28]=[CH:29][CH:30]=1)=[O:7])(=[O:4])=[O:3].[OH-].[Na+].O1CCOCC1>O>[CH3:1][S:2]([NH:5][C:6]([CH2:8][C:9]1[C:10]2[CH2:11][C:12]3[N:17]4[CH:18]=[C:19]([C:21]([OH:23])=[O:22])[N:20]=[C:16]4[C:15](=[O:26])[NH:14][C:13]=3[C:27]=2[CH:28]=[CH:29][CH:30]=1)=[O:7])(=[O:3])=[O:4]

Participants

5

Procedure

The 9-methylsulphonamidocarbonylmethyl-4-oxo-4,5-dihydro-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylic acid can be obtained in the following manner: 4.4 ml of 1 N aqueous sodium hydroxide are added dropwise to a solution of 0.48 g of ethyl 9-methylsulphonamidocarbonylmethyl-4-oxo-4,5-dihydro-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylate, 45 ml of dioxane and 1.3 ml of distilled water. The reaction medium is kept stirring for 20 hours, filtered on sintered glass and the solid thus obtained is washed with twice 20 ml of dioxane, air-dried and then under reduced pressure at 60° C. 0.46 g of 9-methylsulphonamidocarbonylmethyl-4-oxo-4,5-dihydro-10H-imidazo[1,2-a]indeno[1,2-e]pyrazine-2-carboxylic acid is thus obtained as disodium salt in the form of a pink solid melting above 260° C. (Analysis: C17H12N4O6S1Na2, 6.21 H2O, 0.49 C4H8O2, % calculated C: 45.75, H: 2.71, N: 12.55, S: 7.18; % found C: 45.7, H: 2.3, N: 12.5, S: 7.2).

Workup

  1. filtrationfiltered on sintered glass
  2. customthe solid thus obtained
  3. washis washed with twice 20 ml of dioxane
  4. customair-dried
  5. customat 60° C

Sources & evidence

ORD record
ord-c23fdfc2f4d340e5b716900744da854c
Source dataset
uspto-grants-2000_08
Patent number
US06100264

Reaction notes

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