Hydrochloric Acid → HCID 12909281、化合物

HRID 614524ノート

反応式

HRID 614524 の反応式
[CH:1]1[N:9]2[C:4]([CH2:5][O:6][C:7]3[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=32)=[N:3][C:2]=1[C:14]([O:16]C)=[O:15].[OH-].[Na+].Cl>CO.O>[CH:1]1[N:9]2[C:4]([CH2:5][O:6][C:7]3[CH:13]=[CH:12][CH:11]=[CH:10][C:8]=32)=[N:3][C:2]=1[C:14]([OH:16])=[O:15]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12909280HCID 12909280、化合物

生成物 1

HCID 12909281HCID 12909281、化合物収率 91%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

10.0 g (0.0435 mole) of methyl 4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carboxylate were suspended in a mixture of 100 ml of methanol and 50 ml of water and 2N NaOH solution was added to the mixture thus obtained until the pH was 11. The mixture was warmed until the starting material had completely dissolved and thin layer chromatography indicated that no starting material remained. The solution was subsequently acidified to a pH of 2-3 with concentrated hydrochloric acid and the desired product precipitated out. After cooling, the mixture was filtered and the solid product was washed well with water. The white product was dried over P2O5 to obtain 8.5 g (91% yield) of 4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carboxylic acid with a melting point of 256°-8° C. (decarboxylates).

後処理

  1. additionwas added to the mixture
  2. customthus obtained until the pH was 11
  3. temperatureThe mixture was warmed until the starting material
  4. dissolutionhad completely dissolved
  5. customthe desired product precipitated out
  6. temperatureAfter cooling
  7. filtrationthe mixture was filtered
  8. washthe solid product was washed well with water
  9. dry with materialThe white product was dried over P2O5

出典と根拠

ORDレコード
ord-821fa31dac4c4017a7ec2ce1459b7354
出典データセット
uspto-grants-1979_03
特許番号
US04145419

反応ノート

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