Methyl iodide → tert-Butyl Hexahydro-4-methyl-3-oxo-1H-1,4-diazepine-1-carboxylate

HRID 2211834

반응식

HRID 2211834 반응식
[H-].[Na+].[O:3]=[C:4]1[NH:10][CH2:9][CH2:8][CH2:7][N:6]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:5]1.I[CH3:19]>CN(C=O)C.[Cl-].[NH4+]>[CH3:19][N:10]1[CH2:9][CH2:8][CH2:7][N:6]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:5][C:4]1=[O:3]

참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21962087tert-Butyl 3-oxo-1,4-diazepane-1-carboxylate

생성물 1

HCID 21962086tert-Butyl Hexahydro-4-methyl-3-oxo-1H-1,4-diazepine-1-carboxylate

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 25517Ammonium Chloride용매

실험 절차

Sodium hydride (103 mg) was added to a stirred solution of tert-butyl hexahydro-3-oxo-1H-1,4-diazepine-1-carboxylate in DMF (5 mL) at 0° C. After 1 h, iodomethane (0.15 mL) was added, and the resultant mixture was stirred at 0° C., then room temperature overnight. It was diluted with saturated aqueous ammonium chloride solution and extracted with ethyl acetate. The organic layer was separated, washed sequentially with saturated aqueous sodium bicarbonate solution and brine, dried over sodium sulfate, and concentrated to give the product, which was used without further purification.

후처리

  1. customroom temperature overnight
  2. extractionextracted with ethyl acetate
  3. customThe organic layer was separated
  4. washwashed sequentially with saturated aqueous sodium bicarbonate solution and brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated
  7. customto give the product, which
  8. customwas used without further purification

출처 및 근거

ORD 기록
ord-b325bacc98db4c4fa7d085a593171d7f
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07101871B2

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