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Methanol → Methyl 1-amino-4-methoxy-4-(trifluoromethyl)cyclohexanecarboxylate

HRID 922126
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HRID 922126 반응식
[NH2:1][C:2]1([C:14]([OH:16])=[O:15])[CH2:7][CH2:6][C:5]([O:12][CH3:13])([C:8]([F:11])([F:10])[F:9])[CH2:4][CH2:3]1.S(Cl)(Cl)=O.[CH3:21]O>>[NH2:1][C:2]1([C:14]([O:16][CH3:21])=[O:15])[CH2:7][CH2:6][C:5]([O:12][CH3:13])([C:8]([F:11])([F:10])[F:9])[CH2:4][CH2:3]1
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4

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HCID 887MethanolHCID 24386Thionyl Chloride3회HCID 904137291-Amino-4-methoxy-4-(trifluoromethyl)cyclohexanecarboxylic acid

생성물 1

HCID 71246475Methyl 1-amino-4-methoxy-4-(trifluoromethyl)cyclohexanecarboxylate

실험 절차

12.20 g (corresponds to about 37.58 mmol) of 1-amino-4-methoxy-4-(trifluoromethyl)cyclohexanecarboxylic acid (Example 18A) were suspended in 210 ml of methanol, and 10.4 ml (142.80 mmol) of thionyl chloride were added at 0° C. The mixture was boiled under reflux for 2 hours and cooled, another 10.4 ml (142.80 mmol) of thionyl chloride were added at 0° C. and the mixture was boiled under reflux for a further 2 hours. The reaction was cooled, another 10.4 ml (142.80 mmol) of thionyl chloride were added and the mixture was heated at reflux overnight until the reaction had gone to completion. For work-up, about 100 ml of methanol were distilled off and the concentrate was poured into 1 l of saturated aqueous sodium carbonate solution. The product was extracted with ethyl acetate and the organic phase was dried over sodium sulphate. Concentration by evaporation gave 7.01 g (73% of theory) of the title compound as a yellowish oil.

후처리

  1. temperatureunder reflux for 2 hours
  2. temperaturecooled
  3. temperatureunder reflux for a further 2 hours
  4. temperatureThe reaction was cooled
  5. temperaturethe mixture was heated
  6. temperatureat reflux overnight until the reaction
  7. distillationFor work-up, about 100 ml of methanol were distilled off
  8. additionthe concentrate was poured into 1 l of saturated aqueous sodium carbonate solution
  9. extractionThe product was extracted with ethyl acetate
  10. dry with materialthe organic phase was dried over sodium sulphate
  11. concentrationConcentration
  12. customby evaporation

출처 및 근거

ORD 기록
ord-d4e0852c25294342b9351ba61810761f
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09278925B2

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