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Methanol → 1-Methoxy-2,5,9-trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaene

HRID 65466
ノート
印刷プレビュー

反応式

HRID 65466 の反応式
[CH3:1][C:2](=[CH:5][CH:6]=[C:7]([CH3:24])[CH:8]=[CH:9][CH:10]=[C:11]([CH3:23])[CH:12]=[CH:13][C:14]1[C:19]([CH3:21])([CH3:20])[CH2:18][CH2:17][CH2:16][C:15]=1[CH3:22])[CH2:3][OH:4].[CH:25](OC)(OC)OC.CO.FC(F)(F)C(O)=O.C([O-])(O)=O.[Na+]>C1COCC1>[CH3:25][O:4][CH2:3][C:2]([CH3:1])=[CH:5][CH:6]=[C:7]([CH3:24])[CH:8]=[CH:9][CH:10]=[C:11]([CH3:23])[CH:12]=[CH:13][C:14]1[C:19]([CH3:21])([CH3:20])[CH2:18][CH2:17][CH2:16][C:15]=1[CH3:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 887MethanolHCID 6422Trifluoroacetic acidHCID 9005Trimethyl orthoformateHCID 516892Sodium BicarbonateHCID 537496932,5,9-Trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaene-1-ol

生成物 1

HCID 543300171-Methoxy-2,5,9-trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaene

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 2,5,9-trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaene-1-ol (1.6 g, 5 mmol), 1.06 g (10 mmol) of trimethyl orthoformate and 160 mg (5 mmol) of dry methanol in 5 ml of dry THF is added dropwise a solution of 40 μL of trifluoroacetic acid in 1 ml of dry THF over a 1 minute period at room temperature. After overnight standing, the reaction mixture is poured into cold aqueous 5% NaHCO3 and extracted with chloroform three times. The combined organic extract is washed with water, dried over Na2SO4 and evaporated in vacuo to give a residue, which is purified by HPLC (4% ether in hexane, silica gel column) to afford of 1-methoxy-2,5,9-trimethyl-11-(2,6,6-trimethyl-1-cyclohexen-1-yl)-2,4,6,8,10-undecapentaene as an oil.

後処理

  1. extractionextracted with chloroform three times
  2. extractionThe combined organic extract
  3. washis washed with water
  4. dry with materialdried over Na2SO4
  5. customevaporated in vacuo
  6. customto give a residue, which
  7. customis purified by HPLC (4% ether in hexane, silica gel column)

出典と根拠

ORDレコード
ord-901043a06e1f47c9a4918215e06d7b4d
出典データセット
uspto-grants-1986_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04614747

反応ノート

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