Ethanolamine → 2-(2-Ethyl-5-phenyl-1H-pyrrol-1-yl)ethanol

HRID 1824562노트

반응식

HRID 1824562 반응식
[C:1]1([C:7](=O)[CH2:8][CH2:9][C:10](=O)[CH2:11][CH3:12])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH2:15]([CH2:17][NH2:18])[OH:16].C(O)(=O)C(C)(C)C.CCCCCCC.O1CCCC1.C1(C)C=CC=CC=1>ClCCl.O>[OH:16][CH2:15][CH2:17][N:18]1[C:10]([CH2:11][CH3:12])=[CH:9][CH:8]=[C:7]1[C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

7

반응물 4

HCID 700EthanolamineHCID 6417Pivalic acidHCID 110632161-Phenyl-1,4-hexanedioneHCID 22168748HCID 22168748, 화합물

생성물 1

HCID 221687532-(2-Ethyl-5-phenyl-1H-pyrrol-1-yl)ethanol

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 1-phenyl-hexane-1,4-dione (5 g), ethanol amine (1.6 g) and pivalic acid (2.15 g) in a solvent mixture containing n-heptane:tetrahydrofuran:toluene (4:1:1, 50 mL) was refluxed with stirring at 110–120° C. Water formed during the reaction was removed azeotropically during 3 to 4 hrs. The reaction mixture was cooled and the solvent was removed. The residue obtained was dissolved in dichloromethane (50 mL), washed with saturated sodium bicarbonate solution (50 mL), water (50 mL), and then with brine (50 mL), dried (Na2SO4) and the solvent was evaporated. The crude compound obtained as an oily mass. The crude substance was used in the next step without purification.

후처리

  1. temperaturewas refluxed
  2. customwas removed azeotropically during 3 to 4 hrs
  3. temperatureThe reaction mixture was cooled
  4. customthe solvent was removed
  5. customThe residue obtained
  6. washwashed with saturated sodium bicarbonate solution (50 mL), water (50 mL)
  7. dry with materialwith brine (50 mL), dried (Na2SO4)
  8. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-f56ec55032254d69859cd357788247b1
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07041837B2

반응 노트

불러오는 중…