홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Water → 2-(3,4-Dimethoxyphenoxy)ethanol

HRID 1272040
노트
인쇄 미리보기

반응식

HRID 1272040 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([OH:11])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[H-].[Na+].[O:14]1C=CC=[CH:16][CH:15]1OCCBr.O>CC(N(C)C)=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]=[CH:7][C:8]=1[O:9][CH3:10])[O:11][CH2:16][CH2:15][OH:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 162513,4-DimethoxyphenolHCID 24758Sodium hydrideHCID 184563812-(2-Bromoethoxy)-2H-pyran

생성물 1

HCID 122988832-(3,4-Dimethoxyphenoxy)ethanol

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

실험 절차

A mixture of 3,4-dimethoxyphenol (155 mg, 1.0 mmol) and 60% sodium hydride (50 mg, 1.25 mmol) in DMA (6 ml) was stirred for 20 min under an atmosphere of nitrogen. 2-(2-Pyranyloxy)ethylbromide (220 mg, 1.0 mmol) was added dropwise. The reaction mixture was stirred for 6 hours at room temperature and then the mixture was poured into water (100 ml). The mixture was extracted with ethyl acetate (2×30 ml) and the combined organic extracts were dried (MgSO4). The organic phase was concentrated and the residue was dissolved in 2-propanol (30 ml) and 4 N HCl (20 ml) was added. The mixture was heated at reflux temperature for 30 min and then stirred at room temperature for 2 hours. The reaction mixture was concentrated and the residue was dissolved in ethyl acetate (50 ml). The organic solution was dried (MgSO4) and the solvent was evaporated. The oily residue was purified on silica gel (50 g) eluting with a mixture of heptane and ethyl acetate (3:2). This afforded 100 mg (50%) of 2-(3,4-dimethoxyphenoxy)ethanol.

후처리

  1. stirringThe reaction mixture was stirred for 6 hours at room temperature
  2. extractionThe mixture was extracted with ethyl acetate (2×30 ml)
  3. dry with materialthe combined organic extracts were dried (MgSO4)
  4. concentrationThe organic phase was concentrated
  5. dissolutionthe residue was dissolved in 2-propanol (30 ml)
  6. addition4 N HCl (20 ml) was added
  7. temperatureThe mixture was heated
  8. temperatureat reflux temperature for 30 min
  9. stirringstirred at room temperature for 2 hours
  10. concentrationThe reaction mixture was concentrated
  11. dissolutionthe residue was dissolved in ethyl acetate (50 ml)
  12. dry with materialThe organic solution was dried (MgSO4)
  13. customthe solvent was evaporated
  14. customThe oily residue was purified on silica gel (50 g)
  15. washeluting with a mixture of heptane and ethyl acetate (3:2)

출처 및 근거

ORD 기록
ord-85e3ed54eb7c41949095337b1749c24d
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07208497B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트