Potassium Cyanide → 1091611-71-0

HRID 450780ノート

反応式

HRID 450780 の反応式
[C-:1]#[N:2].[K+].O1CCOCCOCCOCCOCCOCC1.Cl[CH2:23][C:24]1[CH:25]=[C:26]([CH:34]=[CH:35][CH:36]=1)[C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28]>C(#N)C>[C:1]([CH2:23][C:24]1[CH:25]=[C:26]([CH:34]=[CH:35][CH:36]=1)[C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])#[N:2]

参加物

5

反応物 3

HCID 9032Potassium CyanideHCID 2855718-Crown-6HCID 22456708tert-Butyl 3-(chloromethyl)benzoate

生成物 1

HCID 594787811091611-71-0収率 80.6%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

実験手順

To a mixed liquid of 1.51 g of potassium cyanide and 70 ml of acetonitrile, 6.12 g of 1,4,7,10,13,16-hexaoxacyclooctadecane was added, followed by stirring for 2 hours. Thereafter, a solution of 5.00 g of tert-butyl 3-(chloromethyl)benzoate in 30 ml of acetonitrile was added thereto, followed by stirring at room temperature for 18 hours. The reaction solution was concentrated, diluted with diethyl ether-hexane (1:1), and then washed with water and a saturated aqueous sodium chloride solution. After drying over anhydrous magnesium sulfate, the solvent was evaporated, and the residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate) to obtain 3.86 g of tert-butyl 3-(cyanomethyl)benzoate as a colorless oily substance.

後処理

  1. stirringby stirring at room temperature for 18 hours
  2. concentrationThe reaction solution was concentrated
  3. additiondiluted with diethyl ether-hexane (1:1)
  4. washwashed with water
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. customthe solvent was evaporated
  7. customthe residue was purified by silica gel column chromatography (eluent: hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-c21fceb80bfe42f7912d7ee557077df2
出典データセット
uspto-grants-2013_07
特許番号
US08486970B2

反応ノート

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