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

Pyridine → HCID 53730792, 화합물

HRID 1488944
노트
인쇄 미리보기

반응식

HRID 1488944 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]#[C:12][C:13]([OH:15])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].S(Cl)([Cl:18])=O.N1C=CC=CC=1.[NH:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1>C1(C)C=CC=CC=1>[Cl:18][C:11]([C:5]1[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=1)=[CH:12][C:13]([N:26]1[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1)=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1049PyridineHCID 8083MorpholineHCID 24386Thionyl ChlorideHCID 37083353-(3,4-Dimethoxy-phenyl)-propynoic acid

생성물 1

HCID 53730792HCID 53730792, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

20.6 g (0.1 mol) of 3-(3,4-Dimethoxyphenyl)prop-2-ynoic acid and 36 ml (0.5 mol) of thionylchloride are stirred at room temperature for 2 hours. The excess thionylchloride is evaporated and the residue dissolved in 50 ml of toluene. This solution is added under ice cooling and stirring to a solution of 50 ml of pyridine and 10.9 g (0.125 mol) of morpholine in 100 ml of toluene. After 10 minutes of further stirring at room temperature the mixture is heated to 90° C. for 10 minutes. The mixture is cooled and then extracted twice with 250 ml of 2N hydrochloric acid and once with water, dried and evaporated. The resulting compound is purified by flash column chromatography using as eluant 1000 ml of toluene/acetone (10 and 20% of acetone). The fractions with Rf-value 0.52 and 0.43 in TLC (toluene/acetone 7:3) are gathered and the solvent is evaporated.

후처리

  1. customThe excess thionylchloride is evaporated
  2. dissolutionthe residue dissolved in 50 ml of toluene
  3. additionThis solution is added under ice cooling
  4. temperatureis heated to 90° C. for 10 minutes
  5. temperatureThe mixture is cooled
  6. extractionextracted twice with 250 ml of 2N hydrochloric acid and once with water
  7. customdried
  8. customevaporated
  9. customThe resulting compound is purified by flash column chromatography
  10. customthe solvent is evaporated

출처 및 근거

ORD 기록
ord-ca7695195cad40b4bac403772abfed94
출처 데이터셋
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05677303

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트