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Tetrahydrofuran → (5Z)-3-methylnon-5-enyl acetate

HRID 2059551
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HRID 2059551 반응식
CC(C)([O-])C.[K+].[C:7]([O:10][CH2:11][CH2:12][CH:13]([CH3:17])[CH2:14][CH:15]=O)(=[O:9])[CH3:8].[CH2:18]1[CH2:22]O[CH2:20][CH2:19]1>[Br-].C([P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)CCC>[C:7]([O:10][CH2:11][CH2:12][CH:13]([CH3:17])[CH2:14]/[CH:15]=[CH:22]\[CH2:18][CH2:19][CH3:20])(=[O:9])[CH3:8]
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참가 물질

5

반응물 3

HCID 8028Tetrahydrofuran3회HCID 110519253-Methyl-5-oxopentyl acetateHCID 23665647Potassium tert-butoxide

생성물 1

HCID 86625206(5Z)-3-methylnon-5-enyl acetate수율 78%

시약·촉매·용매 1

HCID 159628Butyltriphenylphosphonium bromide촉매

실험 절차

Under an atmosphere of nitrogen, a solution of 46.3 g (413 mmol) of potassium tert-butoxide in 250 mL of dry THF was a added between −15° C. and −10° C. to a stirred mixture of 150 g (376 mmol) butyl triphenylphosphonium bromide in 500 mL of dry THF. After complete addition, stirring was continued at −10° C. for 30 min, prior to the dropwise addition of 65.3 g (413 mmol) of 3-methyl-5-oxopentyl acetate in 250 mL of dry THF within a period of 30 min. Stirring was continued a further 15 min at −10° C., before the cooling bath was removed and the reaction mixture was allowed to warm to room temp. After 3 h of stirring at room temp., the reaction mixture was poured into 1 L of water, the organic layer separated and aqueous one extracted twice with 1 L of ether each. The combined organic extracts were washed with water and brine, dried with sodium sulphate, and concentrated under reduced pressure. The crude material (191 g) was purified by flash chromatography (1.00 kg of silica gel, pentane/ether, 19:1, Rf=0.40) to afford 57.9 g (78%) of (5Z)-3-methylnon-5-enyl acetate as a colourless liquid.

후처리

  1. additionAfter complete addition
  2. stirringStirring
  3. waitwas continued a further 15 min at −10° C., before the cooling bath
  4. customwas removed
  5. stirringAfter 3 h of stirring at room temp.
  6. additionthe reaction mixture was poured into 1 L of water
  7. customthe organic layer separated
  8. extractionaqueous one extracted twice with 1 L of ether each
  9. washThe combined organic extracts were washed with water and brine
  10. dry with materialdried with sodium sulphate
  11. concentrationconcentrated under reduced pressure
  12. customThe crude material (191 g) was purified by flash chromatography (1.00 kg of silica gel, pentane/ether, 19:1, Rf=0.40)

출처 및 근거

ORD 기록
ord-bbafd291e0814f8194d482de053075ac
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08278230B2

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