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Diisopropylamine → 1-(4-Benzyloxy-2-tert-butoxycarbonylbutyl)cyclohex-2-ene carboxylic acid

HRID 1459884
ノート
印刷プレビュー

反応式

HRID 1459884 の反応式
C(NC(C)C)(C)C.C([Li])CCC.CCCCCC.[C:19]1([C:25]([OH:27])=[O:26])[CH2:24][CH2:23][CH2:22][CH2:21][CH:20]=1.[C:28]([O:32][C:33](=[O:46])[C:34]([CH2:36][CH2:37][O:38][CH2:39][C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1)=[CH2:35])([CH3:31])([CH3:30])[CH3:29]>O1CCCC1>[CH2:39]([O:38][CH2:37][CH2:36][CH:34]([C:33]([O:32][C:28]([CH3:29])([CH3:31])[CH3:30])=[O:46])[CH2:35][C:19]1([C:25]([OH:27])=[O:26])[CH2:24][CH2:23][CH2:22][CH:21]=[CH:20]1)[C:40]1[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=1
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

7

反応物 5

HCID 7912DiisopropylamineHCID 8058HexaneHCID 694701-Cyclohexene-1-carboxylic acidHCID 539165622-(2-Benzyloxyethyl)acrylic acid tert-butyl esterHCID 178418339Butyllithium

生成物 1

HCID 541070441-(4-Benzyloxy-2-tert-butoxycarbonylbutyl)cyclohex-2-ene carboxylic acid

試薬・触媒・溶媒

1
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-50 °C

実験手順

To a solution of diisopropylamine (8.8 mL, 62.8 mmol) in dry tetrahydrofuran (140 mL) at -50° C. was added a 2.5M solution of n-butyllithium in hexane (25 mL, 12.5 mmol). The mixture was stirred at a temperature from -50° C. to -20° C. over 30 minutes and then cooled again to -50° C. Solid 1-cyclohexene carboxylic acid (3.75 g, 29.7 mmol) was added and the resulting mixture was allowed to warm to room temperature with stirring over 1.5 hours. The reaction was cooled to -78° C. and a solution of 2-(2-benzyloxyethyl)acrylic acid tert-butyl ester (7.45 g, 28.4 mmol) in dry tetrahydrofuran (90 mL) was added over 15 minutes; stirring was continued at -78° C. for 5 hours. The mixture was then allowed to warm to -30° C. over 40 minutes and was quenched by the addition of saturated aqueous NH4Cl solution. After acidification using 3N HCl solution, the mixture was extracted with ether. The extract was washed with brine, dried over MgSO4 and evaporated under vacuum to leave a yellow oil from which 1-(4-benzyloxy-2-tert-butoxycarbonylbutyl)cyclohex-2-ene carboxylic acid (an oily mixture of the two diastereomers), 9.71 g (84%) was isolated by chromatography on silica gel eluting with methylene chloride and then 5% methanol in methylene chloride.

後処理

  1. temperatureto warm to room temperature
  2. stirringwith stirring over 1.5 hours
  3. temperatureThe reaction was cooled to -78° C.
  4. stirringstirring
  5. waitwas continued at -78° C. for 5 hours
  6. temperatureto warm to -30° C. over 40 minutes
  7. customwas quenched by the addition of saturated aqueous NH4Cl solution
  8. extractionthe mixture was extracted with ether
  9. washThe extract was washed with brine
  10. dry with materialdried over MgSO4
  11. customevaporated under vacuum

出典と根拠

ORDレコード
ord-38035244f8d743818a86850635b9494d
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05854275

反応ノート

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