Hydrochloric Acid → HCID 20149487、化合物

HRID 568973ノート

反応式

HRID 568973 の反応式
C1(=O)[N:5]([C:6]([C:30]([O:32][CH2:33][CH3:34])=[O:31])([CH2:12][CH2:13][CH:14]([F:29])[CH:15]([N:18]2C(=O)C3=CC=CC=C3C2=O)[CH:16]=[CH2:17])[C:7]([O:9][CH2:10][CH3:11])=[O:8])C(=O)C2=CC=CC=C12.O1CCOCC1.C(O)C.Cl.C(O)C.N>C(O)C>[NH2:5][C:6]([C:7]([O:9][CH2:10][CH3:11])=[O:8])([CH2:12][CH2:13][CH:14]([F:29])[CH:15]([NH2:18])[CH:16]=[CH2:17])[C:30]([O:32][CH2:33][CH3:34])=[O:31]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 20149438HCID 20149438、化合物HCID 22020343Ethanol, reaction products with ammonia, distn. residuesHCID 22560076Dioxan ethanol

生成物 1

HCID 20149487HCID 20149487、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
90 °C

実験手順

The foregoing compound 22 (17.5 g, 31.8 mmoles) and a 1M solution of N2H4.H2O in dioxane/ethanol 4:1 (35 mL, 2 equivalents) are stirred and heated at about 90° C. After 3 hours, a yellow precipitate is formed, and the mixture is allowed to cool to room temperature. The precipitate is filtered and the filtrate is evaporated to yield an oil. The oil and the precipitate are united and heated with ethanol (310 mL) and conc. HCl (18.6 mL) at 90° C. for 3 hours. After cooling, phthalhydrazide is filtered and the solution is evaporated. Dissolving in water, filtration, evaporation, dissolving in ethanol, evaporating again and drying (oil pump) yields a yellow foam: 11.5 g (about 100%). Thin layer chromatography (ethanol/ammonia 80/20) shows a second spot (presumably some ester cleaved). The compound 23 is utilized for the next step without further purification.

後処理

  1. customa yellow precipitate is formed
  2. temperatureto cool to room temperature
  3. filtrationThe precipitate is filtered
  4. customthe filtrate is evaporated
  5. customto yield an oil
  6. temperatureAfter cooling
  7. filtrationphthalhydrazide is filtered
  8. customthe solution is evaporated
  9. dissolutionDissolving in water
  10. filtrationfiltration, evaporation
  11. dissolutiondissolving in ethanol
  12. customevaporating again
  13. customdrying (oil pump)
  14. customyields a yellow foam
  15. customThe compound 23 is utilized for the next step without further purification

出典と根拠

ORDレコード
ord-855a897586584be5a0c309f2878ebce1
出典データセット
uspto-grants-1988_03
特許番号
US04730006

反応ノート

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