Hydrochloric Acid → HCID 19969538, 화합물

HRID 974856노트

반응식

HRID 974856 반응식
Cl.[OH:2][N:3]=[C:4]([CH2:19][CH:20]([CH3:22])[CH3:21])[C:5]([NH:7][CH:8]([C:14](OCC)=[O:15])[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:6].CN(C)C.B>>[CH2:12]([O:11][C:9]([CH:8]1[NH:7][C:5](=[O:6])[CH:4]([CH2:19][CH:20]([CH3:22])[CH3:21])[N:3]([OH:2])[C:14]1=[O:15])=[O:10])[CH3:13]

참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 2723991N,N-Dimethylmethanamine--borane (1/1)HCID 86747153HCID 86747153, 화합물

생성물 1

HCID 19969538HCID 19969538, 화합물수율 18.6%

실험 절차

240 ml of 7N hydrochloric acid (an ethanolic solution) was dropwise added to 240 ml of an ethanolic solution containing 18.46 g of diethyl N-(2-hydroxyimino-4-methylpentanoyl)aminomalonate and 5.49 g of borane-trimethylamine, with ice-cooling. The mixture was stirred at room temperature for 15 hours. The reaction mixture was subjected to vacuum distillation at room temperature to remove the solvent. The residue was dissolved in dichloromethane. The resulting solution was washed with an aqueous solution saturated with sodium chloride and an aqueous solution saturated with sodium hydrogen carbonate in this order, then dried with anhydrous magnesium sulfate, and was subjected to distillation to remove the solvent. The resulting yellow oily substance was dissolved in 120 ml of toluene. The solution was refluxed for 1 hour and then subjected to distillation to remove the solvent. 19.02 g of the resulting orange oily substance was purified by silica gel column chromatography (eluant: dichloromethane/methanol =30/1) to obtain 2.94 g of 3-ethoxycarbonyl-1-hydroxy-6-isobutylpiperazine-2,5-dione as an orange oily substance.

후처리

  1. temperaturewith ice-cooling
  2. distillationThe reaction mixture was subjected to vacuum distillation at room temperature
  3. customto remove the solvent
  4. dissolutionThe residue was dissolved in dichloromethane
  5. washThe resulting solution was washed with an aqueous solution saturated with sodium chloride
  6. dry with materialan aqueous solution saturated with sodium hydrogen carbonate in this order, then dried with anhydrous magnesium sulfate
  7. distillationwas subjected to distillation
  8. customto remove the solvent
  9. dissolutionThe resulting yellow oily substance was dissolved in 120 ml of toluene
  10. temperatureThe solution was refluxed for 1 hour
  11. distillationsubjected to distillation
  12. customto remove the solvent
  13. custom19.02 g of the resulting orange oily substance was purified by silica gel column chromatography (eluant: dichloromethane/methanol =30/1)

출처 및 근거

ORD 기록
ord-853cb3f5ba3c414eb633f25a2c665213
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05607934

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