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Diethyl Ether → 1-(1-{4-[(1E)-Pent-1-en-1-yl]phenyl}cyclohexyl)methanamine

HRID 2090099
ノート
印刷プレビュー

反応式

HRID 2090099 の反応式
[CH:1](/[C:6]1[CH:11]=[CH:10][C:9]([C:12]2([C:18]#[N:19])[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]2)=[CH:8][CH:7]=1)=[CH:2]\[CH2:3][CH2:4][CH3:5].[H-].[Al+3].[Li+].[H-].[H-].[H-].CCOCC>O1CCCC1>[CH:1](/[C:6]1[CH:11]=[CH:10][C:9]([C:12]2([CH2:18][NH2:19])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17]2)=[CH:8][CH:7]=1)=[CH:2]\[CH2:3][CH2:4][CH3:5]
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 3283Diethyl EtherHCID 21226445Aluminium lithium hydrideHCID 684116391-{4-[(1E)-pent-1-en-1-yl]phenyl}cyclohexanecarbonitrile2 回

生成物 1

HCID 594359221-(1-{4-[(1E)-Pent-1-en-1-yl]phenyl}cyclohexyl)methanamine収率 102.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 1-(4-chlorophenyl)-1-cyclohexanecarbonitrile (100 mg, 0.455 mmol) and 1-pentenylboronic acid (104 mg, 0.910 mmol) in tetrahydrofuran (2 ml) and 1 M potassium carbonate (1.5 ml, 1.500 mmol) was added 1,1′-bis(di t-butylphosphino)ferrocene palladium dichloride (10 mg, 0.056 mmol). The mixture was microwaved at 100° C. in a sealed tube for 20 min, at which point LC/MS analysis showed a new peak. The reaction mixture was diluted with 10 mL of EtOAc and 10 mL of saturated aqueous NaHCO3. The phases were separated and the aqueous phase was extracted with 10 mL of EtOAc. The combined organics were washed with 10 mL of brine, dried (Na2SO4), and concentrated. The residue was purified by flash chromatography on a Biotage Horizon, 25M column, eluting with 1 CV of 100% hexanes followed by a gradient of 0 to 100% EtOAc in hexanes over 10 CV to provide the desired product 1-{4-[(1E)-pent-1-en-1-yl]phenyl}cyclohexanecarbonitrile (83 mg, 0.328 mmol, 72.0% yield). To a 0° C. solution of 1-{4-[(1E)-pent-1-en-1-yl]phenyl}cyclohexanecarbonitrile (75 mg, 0.296 mmol) in tetrahydrofuran (2 ml) was added 1.0 M lithium aluminum hydride in ether (1 ml, 1.000 mmol). The mixture was allowed to warm to room temperature and stirred at this temperature overnight, at which point LC/MS analysis showed complete disappearance of the starting nitrile. The mixture was recooled to 0° C. and quenched by dropwise addition of 30 μl of water, 30 μl of 15% NaOH, and 80 μl of water. The mixture was stirred for 30 min at room temperature, and then filtered, washing the solids liberally with ether. The filtrate was concentrated to provide the title compound (78 mg, 0.303 mmol, 102% yield). Mass spectrum (ESI) 258.0 (M+1).

後処理

  1. customwas recooled to 0° C.
  2. customquenched by dropwise addition of 30 μl of water, 30 μl of 15% NaOH, and 80 μl of water
  3. stirringThe mixture was stirred for 30 min at room temperature
  4. filtrationfiltered
  5. washwashing the solids liberally with ether
  6. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-17cddf13591a4aaa9d85aebecc67c314
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436028B2

反応ノート

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