Sodium Hydroxide → HCID 12909299、化合物

HRID 614528ノート

反応式

HRID 614528 の反応式
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[O:12][CH2:11][C:10]3=[N:13][C:14]([C:16]([O:18][CH3:19])=[O:17])=[CH:15][N:9]3[C:8]=2[CH:20]=1)([O-])=O.[OH-].[Na+]>C(O)(=O)C.Cl>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]2[O:12][CH2:11][C:10]3=[N:13][C:14]([C:16]([O:18][CH3:19])=[O:17])=[CH:15][N:9]3[C:8]=2[CH:20]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 12909298HCID 12909298、化合物

生成物 1

HCID 12909299HCID 12909299、化合物収率 61.2%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒

反応条件

温度
40 °C

実験手順

5.0 g (0.018 mole) of methyl 8-nitro-4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carboxylate were suspended in a mixture of 20 ml of acetic acid and 15 ml of concentrated hydrochloric acid and to the solution thus obtained were added 15 g (0.055 mole) of stannous chloride. The mixture obtained was stirred and warmed to 40° C. After about an hour, a crystalline product started to appear and the mixture was then cooled for two hours in an ice bath. The product (chlorostannate salt) was filtered off and washed with ether. The salt was then dissolved in water and the pH of the solution obtained was adjusted to pH 9 using dilute sodium hydroxide solution. The free amino compound was extracted with chloroform and the combined chloroform extracts were dried, filtered and evaporated. The residue was triturated with ether to obtain 2.7 g (61% yield) of methyl 8-amino-4H-imidazo-[2,1-c][1,4]-benzoxazine-2-carboxylate in the form of brown crystals with a melting point of 213°-4° C.

後処理

  1. customthus obtained
  2. customThe mixture obtained
  3. waitAfter about an hour
  4. temperaturethe mixture was then cooled for two hours in an ice bath
  5. filtrationThe product (chlorostannate salt) was filtered off
  6. washwashed with ether
  7. dissolutionThe salt was then dissolved in water
  8. customthe pH of the solution obtained
  9. extractionThe free amino compound was extracted with chloroform
  10. dry with materialthe combined chloroform extracts were dried
  11. filtrationfiltered
  12. customevaporated
  13. customThe residue was triturated with ether

出典と根拠

ORDレコード
ord-ce86e85794fb4edca26cc0080cbf117a
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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