Water → Benzyl [2-(dimethylcarbamoyl)ethyl]methylcarbamate

HRID 17415

反応式

HRID 17415 の反応式
[CH3:1][N:2]([CH3:18])[C:3]([CH2:5][CH2:6][NH:7][C:8](=[O:17])[O:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:4].[H-].[Na+].I[CH3:22].O>O1CCCC1>[CH3:18][N:2]([CH3:1])[C:3]([CH2:5][CH2:6][N:7]([CH3:22])[C:8](=[O:17])[O:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)=[O:4]

参加物

6

反応物 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 19971000Benzyl [2-(dimethylcarbamoyl)ethyl]carbamate

生成物 1

HCID 69194413Benzyl [2-(dimethylcarbamoyl)ethyl]methylcarbamate収率 86%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Benzyl [2-(dimethylcarbamoyl)ethyl]carbamate (I-139) (0.69 g, 2.76 mmol) was dissolved in tetrahydrofuran (10 ml), and with cooling with ice, sodium hydride (oily, about 55%, 0.15 g, 3.44 mmol) was added, followed by stirring for 10 minutes. Iodomethane (0.26 ml, 4.18 mmol) was added, followed by stirring at room temperature for 18 hours, and water was added. After extraction with ethyl acetate and drying over anhydrous sodium sulfate, the solvent was evaporated away, and the resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=40:1) to obtain a colorless oil (0.63 g, 86%).

後処理

  1. additionwas added
  2. stirringby stirring at room temperature for 18 hours
  3. extractionAfter extraction with ethyl acetate
  4. dry with materialdrying over anhydrous sodium sulfate
  5. customthe solvent was evaporated away
  6. customthe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=40:1)

出典と根拠

ORDレコード
ord-530b116b529646a3ad038a0a1c9fd348
出典データセット
uspto-grants-2010_06
特許番号
US07737166B2

関連ノート

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