Methyl iodide → 3,3-Dimethyl-2,4-pentanedione

HRID 132717

반응식

HRID 132717 반응식
[H-].[Na+].O1CCC[CH2:4]1.[CH3:8][CH:9]([C:13](=[O:15])[CH3:14])[C:10](=[O:12])[CH3:11].IC>O>[CH3:8][C:9]([CH3:4])([C:13](=[O:15])[CH3:14])[C:10](=[O:12])[CH3:11]

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 699493-Methyl-2,4-pentanedione

생성물 1

HCID 765953,3-Dimethyl-2,4-pentanedione수율 98%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To 0.1 mol sodium hydride was added 100 ml anhydrous tetrahydrofuran, and slowly added dropwise 0.12 mol 3-methyl-2,4-pentandione at room temperature. Upon completion, the mixture was stirred for 0.5 hours, then 0.12 mol iodomethane was slowly added dropwise. After stirred at room temperature for 10 hours, 20 ml water was added to dissolve solid. The mixture was extracted with ethyl acetate. The solvent was removed. Distillation was carried out under reduced pressure, and cut fraction 82-84° C./1 kPa was collected. The yield was 98%.

후처리

  1. stirringAfter stirred at room temperature for 10 hours
  2. dissolutionto dissolve solid
  3. extractionThe mixture was extracted with ethyl acetate
  4. customThe solvent was removed
  5. distillationDistillation
  6. customfraction 82-84° C./1 kPa
  7. customwas collected

출처 및 근거

ORD 기록
ord-da4992f5f6e34236ae9e1bcb365f26c5
출처 데이터셋
uspto-grants-2008_06
특허 번호
US07388061B2

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