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

Methyl iodide → 2-(4-Allyloxyphenyl)-2-methylpropionic acid methyl ester

HRID 1443530
노트
인쇄 미리보기

반응식

HRID 1443530 반응식
[CH3:1][O:2][C:3](=[O:16])[CH:4]([C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH:14]=[CH2:15])=[CH:8][CH:7]=1)[CH3:5].[H-].[Na+].[CH3:19]I>CN(C)C=O>[CH3:1][O:2][C:3](=[O:16])[C:4]([C:6]1[CH:7]=[CH:8][C:9]([O:12][CH2:13][CH:14]=[CH2:15])=[CH:10][CH:11]=1)([CH3:19])[CH3:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 685415412-(4-Allyloxyphenyl)-proprionic acid methyl ester

생성물 1

HCID 685403022-(4-Allyloxyphenyl)-2-methylpropionic acid methyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
0 °C

실험 절차

A 0° C. solution of the product of Example 46B (1.9 g, 8.6 mmol) in anhydrous dimethylformamide (10 mL) was treated portion-wise with 60% sodium hydride (410 mg, 10 mmol) in mineral oil. The reaction mixture was stirred twenty minutes at 0° C., and methyl iodide (1.4 mL, 22 mmol) was then added. Ice bath was removed, and reaction mixture stirred 16 hours at room temperature. Reaction mixture quenched with saturated ammonium chloride, and product extracted with ethyl acetate (2×). The combined extracts were washed with water and brine, dried (Na2SO4), filtered, and concentrated under reduced pressure. Residue purified by normal phase HPLC on silica gel eluting with 3% ethyl acetate/hexane to provide the title compound.

후처리

  1. customIce bath was removed
  2. customreaction mixture
  3. stirringstirred 16 hours at room temperature
  4. customReaction mixture
  5. customquenched with saturated ammonium chloride, and product
  6. extractionextracted with ethyl acetate (2×)
  7. washThe combined extracts were washed with water and brine
  8. dry with materialdried (Na2SO4)
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure
  11. customResidue purified by normal phase HPLC on silica gel eluting with 3% ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-5990bf9f63464ce88ae83d0633dae3af
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
USRE041135E1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트