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

HRID 2059551
ノート
印刷プレビュー

反応式

HRID 2059551 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8028Tetrahydrofuran3 回HCID 110519253-Methyl-5-oxopentyl acetateHCID 23665647Potassium tert-butoxide

生成物 1

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

試薬・触媒・溶媒 1

HCID 159628Butyltriphenylphosphonium bromide触媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-bbafd291e0814f8194d482de053075ac
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08278230B2

反応ノート

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