Methyl iodide → Methyl 1-((tert-butoxycarbonyl)amino)-4-oxocyclohexanecarboxylate

HRID 1619495ノート

反応式

HRID 1619495 の反応式
[C:1](=O)([O-])[O-].[K+].[K+].CI.[C:9]([O:13][C:14]([NH:16][C:17]1([C:24]([OH:26])=[O:25])[CH2:22][CH2:21][C:20](=[O:23])[CH2:19][CH2:18]1)=[O:15])([CH3:12])([CH3:11])[CH3:10]>CN(C)C=O>[C:9]([O:13][C:14]([NH:16][C:17]1([C:24]([O:26][CH3:1])=[O:25])[CH2:22][CH2:21][C:20](=[O:23])[CH2:19][CH2:18]1)=[O:15])([CH3:12])([CH3:10])[CH3:11]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 247297681-(((Tert-butoxy)carbonyl)amino)-4-oxocyclohexane-1-carboxylic acid

生成物 1

HCID 57190358Methyl 1-((tert-butoxycarbonyl)amino)-4-oxocyclohexanecarboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3.90 g potassium carbonate and 1.30 ml methyl iodide are added to 4.65 g 1-tert.-butoxycarbonylamino-4-oxo-cyclohexanecarboxylic acid in 45 ml N,N-dimethylformamide and the reaction mixture is stirred for three hours at ambient temperature. Then the solvent is distilled off using the rotary evaporator and the residue is divided between 10% potassium carbonate solution and diethyl ether. The aqueous phase is separated off and extracted with diethyl ether and the combined organic phases are washed with saturated sodium chloride solution, dried on magnesium sulphate and evaporated down. A colourless oil is left, which slowly crystallises.

後処理

  1. distillationThen the solvent is distilled off
  2. customthe rotary evaporator
  3. customThe aqueous phase is separated off
  4. extractionextracted with diethyl ether
  5. washthe combined organic phases are washed with saturated sodium chloride solution
  6. customdried on magnesium sulphate
  7. customevaporated down
  8. waitA colourless oil is left
  9. customwhich slowly crystallises

出典と根拠

ORDレコード
ord-6731bbd97cfb497199a6ba0abccd92ac
出典データセット
uspto-grants-2014_07
特許番号
US08772298B2

反応ノート

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