Hydrochloric Acid → HCID 12909281, 화합물

HRID 614524노트

반응식

HRID 614524 반응식
[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]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12909280HCID 12909280, 화합물

생성물 1

HCID 12909281HCID 12909281, 화합물수율 91%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-821fa31dac4c4017a7ec2ce1459b7354
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04145419

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