Sodium Hydroxide → HCID 18790664、化合物

HRID 1107046ノート

反応式

HRID 1107046 の反応式
[OH-].[Na+].[CH3:3][NH:4][C:5]([CH2:7][C:8]1[C:9]2[CH2:10][C:11]3[N:16]4[CH:17]=[C:18]([C:20]([O:22]CC)=[O:21])[N:19]=[C:15]4[C:14](=[O:25])[NH:13][C:12]=3[C:26]=2[CH:27]=[CH:28][CH:29]=1)=[O:6]>O1CCOCC1>[CH3:3][NH:4][C:5]([CH2:7][C:8]1[C:9]2[CH2:10][C:11]3[N:16]4[CH:17]=[C:18]([C:20]([OH:22])=[O:21])[N:19]=[C:15]4[C:14](=[O:25])[NH:13][C:12]=3[C:26]=2[CH:27]=[CH:28][CH:29]=1)=[O:6]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 18790720HCID 18790720、化合物

生成物 1

HCID 18790664HCID 18790664、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

8.2 ml of 1N sodium hydroxide solution are added dropwise, under a stream of nitrogen and at a temperature in the region of 20° C., to a suspension of 1 g of ethyl 9-(N-methylaminocarbonylmethyl)-4,5-dihydro-4-oxo-10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-2-carboxylate in a dioxane distilled water (100/27 by volume) mixture. The reaction is continued for 2 hours at the same temperature. The light-grey insoluble material is filtered, washed with acetone and then taken up in 15 ml of distilled water. This aqueous solution is filtered and then acidified to pH 1 with N hydrochloric acid. The precipitate formed is filtered and washed with water, with acetone and then with ethyl ether to result in 0.59 g of the trihydrate of 9-(N-methylaminocarbonylmethyl)-4,5-dihydro-4-oxo-10H-imidazo[1,2-a]indeno[1,2-e]pyrazin-2-carboxylic acid in the form of a white powder, the melting point of which is greater than 260° C. (Analysis C17H14N4O4.3H2O; % Calculated C: 60.35, H: 4.17, N: 16.56; % Found C: 60.0, H: 4.1, N: 16.3; 1H NMR spectrum in CD3CO2D, T=300 K, δ in ppm (300 MHz): 2.7 (3H, s, NCH3), 3.9 (2H, , CH2CO), 4.1 (2H, s, CH2), 7.2 (1H, d, J=8 Hz, arom. CH), 7.4 (1H, t, J=8 Hz, arom. CH), 7.7 (1H, d, J=8 Hz, arom. CH), 8.5 (1H, s, imidazole H)).

後処理

  1. distillationdistilled water (100/27 by volume) mixture
  2. filtrationThe light-grey insoluble material is filtered
  3. washwashed with acetone
  4. filtrationThis aqueous solution is filtered
  5. customThe precipitate formed
  6. filtrationis filtered
  7. washwashed with water, with acetone

出典と根拠

ORDレコード
ord-080c730491e24f6bae0876f448284376
出典データセット
uspto-grants-2000_05
特許番号
US06057454

反応ノート

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