Methyl iodide → HCID 67711340, 화합물

HRID 974860노트

반응식

HRID 974860 반응식
[H-].[Na+].[CH2:3]([O:5][C:6]([CH:8]1[NH:13][C:12](=[O:14])[CH:11]([CH2:15][CH:16]([CH3:18])[CH3:17])[N:10]([O:19][CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][O:21]2)[C:9]1=[O:26])=[O:7])[CH3:4].[CH3:27]I.[Cl-].[NH4+]>CN(C)C=O>[CH2:3]([O:5][C:6]([C:8]1([CH3:27])[NH:13][C:12](=[O:14])[CH:11]([CH2:15][CH:16]([CH3:18])[CH3:17])[N:10]([O:19][CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][O:21]2)[C:9]1=[O:26])=[O:7])[CH3:4]

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 19969552HCID 19969552, 화합물

생성물 1

HCID 67711340HCID 67711340, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1.04 g of 60% sodium hydride was added to 100 ml of 9.67 g of 3-ethoxycarbonyl-6-isobutyl-1-(2-tetrahydropyranyloxy)piperazine-2,5-dione in anhydrous N,N-dimethylformamide, on ice cooling, and the mixture was stirred for 10 minutes. Thereto was added 3.5 ml of methyl iodide. The mixture was stirred at room temperature for 5 hours. The reaction mixture was ice-cooled and poured into an aqueous solution saturated with ammonium chloride. The mixture was extracted with ethyl acetate. The extract was washed three times with an aqueous solution saturated with sodium chloride, dried with anhydrous magnesium sulfate, and subjected to distillation to remove the solvent to obtain 8.53 g of (3RS,6SR)-3-ethoxycarbonyl-6-isobutyl-3-methyl-1-(2-tetrahydropyranyloxy)piperazine-2,5-dione as a brown oily substance.

후처리

  1. stirringThe mixture was stirred at room temperature for 5 hours
  2. temperaturecooled
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe extract was washed three times with an aqueous solution saturated with sodium chloride
  5. dry with materialdried with anhydrous magnesium sulfate
  6. distillationsubjected to distillation
  7. customto remove the solvent

출처 및 근거

ORD 기록
ord-129dbc3c4365457083ae4e7b63dc04b8
출처 데이터셋
uspto-grants-1997_03
특허 번호
US05607934

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