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

Sodium hydride → 2-Methyl-alpha-[[4-(tetradecyloxy)phenyl]methyl]-1,3-dioxolane-2-propanoic acid, ethyl ester

HRID 235703
노트
인쇄 미리보기

반응식

HRID 235703 반응식
Br[CH2:2][C:3]1[CH:8]=[CH:7][C:6]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])=[CH:5][CH:4]=1.[CH2:24]1[O:36][C:27]([CH3:35])([CH2:28][CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31])[O:26][CH2:25]1.[H-].[Na+]>O1CCCC1>[CH3:35][C:27]1([CH2:28][CH:29]([CH2:2][C:3]2[CH:8]=[CH:7][C:6]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])=[CH:5][CH:4]=2)[C:30]([O:32][CH2:33][CH3:34])=[O:31])[O:26][CH2:25][CH2:24][O:36]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 70332Ethyl 2-methyl-1,3-dioxolane-2-propionateHCID 100228401-(Bromomethyl)-4-(tetradecyloxy)benzene

생성물 1

HCID 867412682-Methyl-alpha-[[4-(tetradecyloxy)phenyl]methyl]-1,3-dioxolane-2-propanoic acid, ethyl ester수율 52.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of about 33 g of 1-(bromomethyl)-4-(tetradecyloxy)benzene, about 16.2 g of ethyl levulinate ethylene ketal, about 4.54 g of about 50% sodium hydride and about 350 ml of tetrahydrofuran was refluxed with stirring, under argon for about 18 hours and then filtered through celite. The solvent was removed and the residue was dissolved in ether. The ether solution was washed with aqueous monobasic sodium phosphate, dried and the solvent removed. The residue was subjected to high performance liquid chromatography (HPLC), using the system hexane:ethyl acetate (about 9:1), giving about 22.1 g of the desired title compound as a light yellow oil).

후처리

  1. temperaturewas refluxed
  2. filtrationfiltered through celite
  3. customThe solvent was removed
  4. dissolutionthe residue was dissolved in ether
  5. washThe ether solution was washed with aqueous monobasic sodium phosphate
  6. customdried
  7. customthe solvent removed

출처 및 근거

ORD 기록
ord-95bfe5bf32f649c2b074aa3df909609f
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04640913

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트