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Acetic Acid → Ethyl (2E,4E,6E,10E)-3,7,11,15-tetramethylhexadeca-2,4,6,10,14-pentaenoate

HRID 1611064
ノート
印刷プレビュー

反応式

HRID 1611064 の反応式
[O-:1][CH2:2][CH3:3].[Na+].[CH2:5]([C:7]([CH2:20]C)(P(O)(O)=O)/[C:8](/C)=C(\CC)/C([O-])=O)[CH3:6].[CH3:22][C:23]([CH3:37])=[CH:24][CH2:25][CH2:26]/[C:27](/[CH3:36])=[CH:28]/[CH2:29][CH2:30]/[C:31](/[CH3:35])=[CH:32]/[CH:33]=[O:34].C(O)(=O)C>CN(C)C=O>[CH2:2]([O:1][C:33](=[O:34])/[CH:32]=[C:31](\[CH3:35])/[CH:30]=[CH:29]/[CH:28]=[C:27](\[CH3:36])/[CH2:26][CH2:25]/[CH:24]=[C:23](\[CH3:37])/[CH2:22][CH2:6][CH:5]=[C:7]([CH3:20])[CH3:8])[CH3:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 2723922Sodium ethoxideHCID 5280598(2E,6E)-3,7,11-trimethyldodeca-2,6,10-trienalHCID 86584517Triethyl-3-methyl-4-phosphonocrotonate

生成物 1

HCID 11984134Ethyl (2E,4E,6E,10E)-3,7,11,15-tetramethylhexadeca-2,4,6,10,14-pentaenoate収率 88%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒
3 回

反応条件

温度
-10 °C

実験手順

Under argon atmosphere, sodium ethoxide (2.16 g, 1.26 equivalents) was suspended in 20 ml of dimethylformamide, and the suspension was added dropwise with 5 ml dimethylformamide solution of triethyl-3-methyl-4-phosphonocrotonate (7.87 g, 1.2 equivalents, 23.28 mmol) at room temperature. The reaction mixture was then added dropwise with 5 ml dimethylformamide solution of farnesal (5.0 g, 22.7 ml) under stirring at −10° C., and further stirred at the same temperature for 30 minutes. The reaction mixture was added to ice-water. The solution was neutralized with acetic acid and extracted with n-heptane. The resulting organic layer was washed with saturated brine and dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 6.6 g of the title compound (yield 88%, 2E:2Z=86:14) as a yellow oil.

後処理

  1. stirringfurther stirred at the same temperature for 30 minutes
  2. extractionextracted with n-heptane
  3. washThe resulting organic layer was washed with saturated brine
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-96cd9e35864f46eeb81d6aac8379ca43
出典データセット
uspto-grants-2006_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06984742B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート