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

Triethylamine → 4-(2,4-Dimethoxyphenyl)pyridine-2,6-dicarboxylic Acid

HRID 5553
노트
인쇄 미리보기

반응식

HRID 5553 반응식
BrCC1C=C(CBr)C=C(CBr)C=1.CCN(CC)CC.C[O:21][C:22]([C:24]1[CH:29]=[C:28]([C:30]2[CH:35]=[C:34](S(Cl)(=O)=O)[C:33]([O:40][CH3:41])=[CH:32][C:31]=2[O:42][CH3:43])[CH:27]=[C:26]([C:44]([O:46]C)=[O:45])[N:25]=1)=[O:23].C(NCCO)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>C(Cl)Cl.CO.C(Cl)(Cl)Cl.O>[CH3:43][O:42][C:31]1[CH:32]=[C:33]([O:40][CH3:41])[CH:34]=[CH:35][C:30]=1[C:28]1[CH:27]=[C:26]([C:44]([OH:46])=[O:45])[N:25]=[C:24]([C:22]([OH:23])=[O:21])[CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 8471TriethylamineHCID 5302581,3,5-Tris(bromomethyl)benzene2회HCID 31256082-((Triphenylmethyl)amino)ethanolHCID 150019164-(5-Chlorosulfonyl-2,4-dimethoxyphenyl)-2,6-pyridine dicarboxylic acid dimethyl ester

생성물 1

HCID 150019144-(2,4-Dimethoxyphenyl)pyridine-2,6-dicarboxylic Acid

시약·촉매·용매 3

HCID 962
Water
용매
HCID 6344Dichloromethane용매2회
HCID 21584188Chloroform methanol용매

실험 절차

To a suspension of 0.5 g (0.0008 mole) of the amine-hydrochloride 8 in 20 ml of CH2Cl2 was added all at once 1.4 ml (0.01 mole) of Et3N. The mixture was then cooled to 5°-10° C. and 1.4 g (0.0032 mole) of the sulfonyl chloride 39 in 20 ml of CH2Cl2 was slowly added in a dropwise fashion. The reaction was then allowed to stir at room temperature for 30 minutes after which a TLC was taken. Little of the sulfonyl chloride 9 had reacted by TLC so an additional 100 mg of the amine 8 was added and stirring continued overnight. The mixture was then poured into water and extracted with CH2Cl2. The extract was washed with water, dried (Na2SO4) and the solvent removed yielding crude 43. After column chromatography with SiO2 /5%MeOH/CHCl3, 1.55 g (93%) of the desired tetraamide 43 was obtained.

후처리

  1. temperatureThe mixture was then cooled to 5°-10° C.
  2. additionwas added
  3. stirringstirring continued overnight
  4. extractionextracted with CH2Cl2
  5. washThe extract was washed with water
  6. dry with materialdried (Na2SO4)
  7. customthe solvent removed
  8. customyielding crude 43

출처 및 근거

ORD 기록
ord-1c4af60950e34e5ba3caea2d9484da0b
출처 데이터셋
uspto-grants-1993_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05245038

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트