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

Potassium Hydroxide → Ethyl 2-(4-methoxyphenyl)cyclopropanecarboxylate

HRID 922220
노트
인쇄 미리보기

반응식

HRID 922220 반응식
[I-].[CH3:2][S+](C)(C)=O.[OH-].[K+].[CH3:9][O:10][C:11]1[CH:16]=[CH:15][C:14](/[CH:17]=[CH:18]\[C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:13][CH:12]=1>CS(C)=O>[CH3:9][O:10][C:11]1[CH:12]=[CH:13][C:14]([CH:17]2[CH2:2][CH:18]2[C:19]([O:21][CH2:22][CH3:23])=[O:20])=[CH:15][CH:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 74498Sulfoxonium, trimethyl-, iodide (1:1)HCID 13010829Npc140395

생성물 1

HCID 244562Ethyl 2-(4-methoxyphenyl)cyclopropanecarboxylate수율 43.22%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
0 °C

실험 절차

To a 50 mL RB flask fitted with magnetic stirrer was charged with 14 mL of dimethylsulfoxide. To the stirred solvent was added trimethylsulfoxonium iodide (1.53 g, 6.93 mmol). The reaction mixture was cooled to 0° C. and powdered potassium hydroxide (0.42 g, 7.49 mmol) was added portion wise, stirred for 10 minutes at room temperature. Then ethyl (2Z)-3-(4-methoxyphenyl)-acrylate (1.3 g, 6.31 mmol) was added. The reaction mixture was stirred at room temperature for 3 h. The reaction mixture was quenched with water and diethyl ether was added. The layers were separated and the organic layer was washed with brine solution (50 mL). The organic layer was dried over anhydrous Na2SO4 and the solvent was removed under reduced pressure. The crude material was purified by silica gel column chromatography using ethyl acetate and petroleum ether as elutant. The product was obtained as pale pink solid (0.6 g, yield: 43.22%). 1H NMR (300 MHz, CDCl3): δ 6.95-6.98 (d, 2H), 6.74-6.77 (d, 2H), 4.06-4.13 (q, 2H), 3.72 (s, 3H), 2.38-2.44 (m, 1H), 1.72-1.78 (m, 1H), 1.43-1.61 (m, 2H), 1.25-1.29 (t, 3H).

후처리

  1. customTo a 50 mL RB flask fitted with magnetic stirrer
  2. stirringThe reaction mixture was stirred at room temperature for 3 h
  3. customThe reaction mixture was quenched with water and diethyl ether
  4. additionwas added
  5. customThe layers were separated
  6. washthe organic layer was washed with brine solution (50 mL)
  7. dry with materialThe organic layer was dried over anhydrous Na2SO4
  8. customthe solvent was removed under reduced pressure
  9. customThe crude material was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-a4bad09cb0c045ae9f6b7654175e2c1f
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278915B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트