Water → methyl N-methoxy-N-propargylcarbamate

HRID 3402

반응식

HRID 3402 반응식
[H-].[Na+].[CH3:3][O:4][NH:5][C:6](=[O:9])[O:7][CH3:8].[CH2:10](Br)[C:11]#[CH:12].O>O1CCCC1>[CH3:3][O:4][N:5]([CH2:12][C:11]#[CH:10])[C:6](=[O:9])[O:7][CH3:8]

참가 물질

6

반응물 4

HCID 962WaterHCID 7842Propargyl bromideHCID 24758Sodium hydrideHCID 12663380methyl N-methoxycarbamate

생성물 1

HCID 18935021methyl N-methoxy-N-propargylcarbamate수율 58.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

0.43 g of sodium hydride (60% in oil) was suspended in 10 ml of tetrahydrofuran, and 1.0 g of methyl N-methoxycarbamate and 1.36 g of propargyl bromide were added to the suspension in this order while being cooled with ice. The mixture was heat-refluxed for 4 hours. After completion of the reaction, water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The extract was dried, concentrated and purified by silica gel column chromatography to obtain 0.8 g of methyl N-methoxy-N-propargylcarbamate.

후처리

  1. temperaturewhile being cooled with ice
  2. temperatureThe mixture was heat-refluxed for 4 hours
  3. additionwas added to the reaction solution
  4. extractionthe mixture was extracted with ethyl acetate
  5. customThe extract was dried
  6. concentrationconcentrated
  7. custompurified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-cf112f9f981e4357be02e4ddbd112b54
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05733935

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