1-Iodopropane → HCID 69129839, 화합물

HRID 478641노트

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HRID 478641 반응식
[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:9]=[CH:8][C:7]([CH:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)=[CH:6][CH:5]=1.C(N(C(C)C)[CH:20]([CH3:22])[CH3:21])C.ICCC>COCCOC>[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:5]=[CH:6][C:7]([CH:10]2[CH2:15][CH2:14][N:13]([CH2:21][CH2:20][CH3:22])[CH2:12][CH2:11]2)=[CH:8][CH:9]=1

참가 물질

5

반응물 3

HCID 336431-IodopropaneHCID 81531DiisopropylethylamineHCID 24904226Methyl 4-(piperidin-4-yl)benzoate

생성물 1

HCID 69129839HCID 69129839, 화합물

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
70 °C

실험 절차

4-Piperidin-4-yl-benzoic acid methyl ester (28 mmol), ethyldiisopropylamine (31 mol) and 1-iodopropane (42 mmol) are dissolved in 1,2-dimethoxyethane (100 ml) and the mixture is heated at 70° C. overnight. After evaporation of the solvent, the residue is dissolved in a mixture of water and sodium carbonate (to ensure basic conditions) and extracted three times with ethyl acetate. The combined extract is dried over sodium sulfate and evaporated. The residue is purified by flash chromatography on silica gel with CH2Cl2/MeOH=9:1 as mobile phase. The product containing fractions are combined and evaporated. The residue is suspended in diethylether and the solid filtered of and dried (vacuum). A pale brown powder with Rf=0.35 (CH2Cl2/MeOH=9:1) is obtained.

후처리

  1. customAfter evaporation of the solvent
  2. dissolutionthe residue is dissolved in a mixture of water and sodium carbonate (to ensure basic conditions)
  3. extractionextracted three times with ethyl acetate
  4. extractionThe combined extract
  5. dry with materialis dried over sodium sulfate
  6. customevaporated
  7. customThe residue is purified by flash chromatography on silica gel with CH2Cl2/MeOH=9:1 as mobile phase
  8. additionThe product containing fractions
  9. customevaporated
  10. filtrationthe solid filtered of and
  11. customdried (vacuum)
  12. customA pale brown powder with Rf=0.35 (CH2Cl2/MeOH=9:1) is obtained

출처 및 근거

ORD 기록
ord-721fcd3d612a4e6daf66e05989905e19
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06642239B2

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