Methyl iodide → 3,6-Dimethylheptane-2,4-dione

HRID 132738

반응식

HRID 132738 반응식
[H-].[Na+].O1CCC[CH2:4]1.[CH3:8][CH:9]([CH3:17])[CH2:10][C:11](=[O:16])[CH2:12][C:13](=[O:15])[CH3:14].IC>O>[CH3:4][CH:12]([C:11](=[O:16])[CH2:10][CH:9]([CH3:17])[CH3:8])[C:13](=[O:15])[CH3:14]

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 763542,4-Heptanedione, 6-methyl-

생성물 1

HCID 5382833,6-Dimethylheptane-2,4-dione수율 94%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 0.1 mol sodium hydride was added 100 ml anhydrous tetrahydrofuran, then added slowly dropwise 0.1 mol 6-methyl-2,4-heptandione at room temperature. The reaction was stirred for 0.5 hours, then 0.12 mol iodomethane was added dropwise and the reaction was stirred at room temperature for further 10 hours. Upon completing the reaction, 20 ml water was added. The mixture was extracted with ethyl acetate. After removing the solvent, distillation under reduced pressure gave a cut fraction 88-9° C./1 kPa (165-166° C. at atmosphere pressure), and the yield was 94%.

후처리

  1. stirringthe reaction was stirred at room temperature for further 10 hours
  2. additionwas added
  3. extractionThe mixture was extracted with ethyl acetate
  4. customAfter removing
  5. distillationthe solvent, distillation under reduced pressure
  6. customgave a cut fraction 88-9° C./1 kPa (165-166° C. at atmosphere pressure)

출처 및 근거

ORD 기록
ord-bd5b8d7ad93241e686914bdcd1e363f5
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388061B2

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