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

HRID 1824562ノート

反応式

HRID 1824562 の反応式
[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

参加物

7

反応物 4

HCID 700EthanolamineHCID 6417Pivalic acidHCID 110632161-Phenyl-1,4-hexanedioneHCID 22168748HCID 22168748、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f56ec55032254d69859cd357788247b1
出典データセット
uspto-grants-2006_05
特許番号
US07041837B2

反応ノート

読み込み中…