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

4-Methoxy cinnamic acid → N-[2-(4-Chloro-2-methoxyphenyl)-4-methylthiazol-5-yl]-3-(4-methoxyphenyl)acrylamide

HRID 1498952
노트
인쇄 미리보기

반응식

HRID 1498952 반응식
[CH3:1][O:2][C:3]1[CH:13]=[CH:12][C:6]([CH:7]=[CH:8][C:9]([OH:11])=O)=[CH:5][CH:4]=1.S(Cl)(Cl)=O.[NH2:18][C:19]1[S:23][C:22]([C:24]2[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][C:25]=2[O:31][CH3:32])=[N:21][C:20]=1[CH3:33]>N1C=CC=CC=1>[Cl:30][C:27]1[CH:28]=[CH:29][C:24]([C:22]2[S:23][C:19]([NH:18][C:9](=[O:11])[CH:8]=[CH:7][C:6]3[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:13][CH:12]=3)=[C:20]([CH3:33])[N:21]=2)=[C:25]([O:31][CH3:32])[CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 132454-Methoxy cinnamic acidHCID 24386Thionyl ChlorideHCID 686418935-Amino-2-(4-chloro-2-methoxyphenyl)-4-methylthiazole

생성물 1

HCID 77387369N-[2-(4-Chloro-2-methoxyphenyl)-4-methylthiazol-5-yl]-3-(4-methoxyphenyl)acrylamide수율 13%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

4-Methoxycinnamic acid (178 mg, 1.0 mmol) and thionyl chloride (480 mg, 4.0 mmol) were heated under reflux for 2 hours. The excess thionyl chloride was distilled off. The resulting residue was dissolved in pyridine (1 ml). Under an ice cooling, the resulting solution was added to a solution of 5-amino-2-(4-chloro-2-methoxyphenyl)-4-methylthiazole (254 mg, 1.0 mmol) prepared in the Step 28-1-2 in pyridine (4 ml). After the removal of the ice bath, the mixture was stirred for 16 hours at a room temperature. To the mixture, 3.5% hydrochloric acid was added, and the resulting mixture was subjected to extraction with chloroform. The extract was washed with water. The washed product was dried over anhydrous magnesium sulfate, and the solvent was distilled off. The resulting residue was purified by silica gel column chromatography (chloroform:methanol=30:1) to give the title compound (54 mg, 13%).

후처리

  1. temperatureunder reflux for 2 hours
  2. distillationThe excess thionyl chloride was distilled off
  3. dissolutionThe resulting residue was dissolved in pyridine (1 ml)
  4. customAfter the removal of the ice bath
  5. additionTo the mixture, 3.5% hydrochloric acid was added
  6. extractionthe resulting mixture was subjected to extraction with chloroform
  7. washThe extract was washed with water
  8. dry with materialThe washed product was dried over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off
  10. customThe resulting residue was purified by silica gel column chromatography (chloroform:methanol=30:1)

출처 및 근거

ORD 기록
ord-1aa6afc00a204a6eaaf7b1857ad70693
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09200008B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트