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

Ethyl Acetate → 2-[{2-(1,3-Benzodioxol-5-yl)ethyl}dithio]ethyl nicotinate

HRID 1195292
노트
인쇄 미리보기

반응식

HRID 1195292 반응식
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH2:11][S:12][S:13][CH2:14][CH2:15][OH:16])=[CH:9][C:4]=2[O:3][CH2:2]1.Cl.[CH2:18](Cl)[C:19]1[CH:24]=[CH:23][CH:22]=[N:21][CH:20]=1.C(=O)([O-])[OH:27].[Na+].C(OCC)(=O)C>N1C=CC=CC=1.C1C=CC=CC=1>[C:18]([O:16][CH2:15][CH2:14][S:13][S:12][CH2:11][CH2:10][C:8]1[CH:7]=[CH:6][C:5]2[O:1][CH2:2][O:3][C:4]=2[CH:9]=1)(=[O:27])[C:19]1[CH:24]=[CH:23][CH:22]=[N:21][CH:20]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 8857Ethyl AcetateHCID 233943-(Chloromethyl)pyridine hydrochlorideHCID 516892Sodium BicarbonateHCID 190016232-[{2-(1,3-Benzodioxol-5-yl)ethyl}dithio]ethanol

생성물 1

HCID 190016562-[{2-(1,3-Benzodioxol-5-yl)ethyl}dithio]ethyl nicotinate

시약·촉매·용매 2

HCID 241
Benzene
용매
HCID 1049Pyridine용매

실험 절차

4 g of the 2-[{2-(1,3-benzodioxol-5-yl)ethyl}-dithio] ethanol prepared in Example 1 was dissolved in a mixture comprising 20 ml of pyridine and 50 ml of benzene to obtain a solution. 4 g of nicotinyl chloride hydrochloride was added to the solution. The obtained mixture was heated under reflux for 2 hours and poured into ice/water. The obtained mixture was weekly basified with sodium hydrogencarbonate. Ethyl acetate was added to the mixture to carry out the phase separation. The ethyl acetate layer was washed with water five times, dried over anhydrous sodium sulfate and distilled to remove the solvent. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=3:1) to obtain 5.4 g of the title compound as a colorless oil.

후처리

  1. customto obtain a solution
  2. temperatureThe obtained mixture was heated
  3. temperatureunder reflux for 2 hours
  4. customthe phase separation
  5. washThe ethyl acetate layer was washed with water five times
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationdistilled
  8. customto remove the solvent
  9. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-5b9626b2706446feaf0a96b8a89318e4
출처 데이터셋
uspto-grants-1992_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05110956

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트