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

HRID 455909노트

반응식

HRID 455909 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ff9796a59a6f44e39b2b85b0fa8022bb
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08497369B2

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