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

HRID 17415

반응식

HRID 17415 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-530b116b529646a3ad038a0a1c9fd348
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

연결된 노트

불러오는 중…