Tetrahydrofuran → Ethyl 3-(2-anilinothiazol-4-yl)acrylate

HRID 2107265노트

반응식

HRID 2107265 반응식
[NH:1]([C:8]1[S:9][CH:10]=[C:11]([CH:13]=O)[N:12]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:15]([O:17][C:18]([CH:20]=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)=[O:19])[CH3:16].O1CCCC1>O>[NH:1]([C:8]1[S:9][CH:10]=[C:11]([CH:13]=[CH:20][C:18]([O:17][CH2:15][CH3:16])=[O:19])[N:12]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 70670Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl esterHCID 150535702-Anilinothiazole-4-carbaldehyde

생성물 1

HCID 54052926Ethyl 3-(2-anilinothiazol-4-yl)acrylate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

A mixture comprising 3.5 g of 2-anilinothiazole-4-carbaldehyde, 6.5 g of (ethoxycarbonylmethylene)triphenylphosphorane and 35 ml of tetrahydrofuran was heated at 60 ° C. for 2 hours. The reaction mixture was poured into water and extracted with benzene. The benzene extract was dried over anhydrous sodium sulfate, and the solvent was evaporated off under reduced pressure, giving an oil. This oil was purified by silica gel column chromatography. using as eluent a 9:1 mixture of benzene and ethyl acetate, giving the desired compound as yellow crystals.

후처리

  1. extractionextracted with benzene
  2. extractionThe benzene extract
  3. dry with materialwas dried over anhydrous sodium sulfate
  4. customthe solvent was evaporated off under reduced pressure
  5. customgiving an oil
  6. customThis oil was purified by silica gel column chromatography
  7. additiona 9:1 mixture of benzene and ethyl acetate

출처 및 근거

ORD 기록
ord-7f3200267c1946fc93d2bec920aa06e4
출처 데이터셋
uspto-grants-1990_06
특허 번호
US04933355

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