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

HRID 2211834

反応式

HRID 2211834 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 25517Ammonium Chloride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b325bacc98db4c4fa7d085a593171d7f
出典データセット
uspto-grants-2006_09
特許番号
US07101871B2

関連ノート

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