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Trifluoroacetic acid → HCID 178502668, 화합물

HRID 480379
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HRID 480379 반응식
[CH3:1][O:2][N:3]([CH3:31])[C:4](=[O:30])[C:5]1[CH:10]=[CH:9][C:8]([CH2:11][N:12](C(OC(C)(C)C)=O)[C@H:13]2[CH2:18][CH2:17][C@H:16]([C:19]([CH3:22])([CH3:21])[CH3:20])[CH2:15][CH2:14]2)=[CH:7][CH:6]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[CH3:1][O:2][N:3]([CH3:31])[C:4](=[O:30])[C:5]1[CH:6]=[CH:7][C:8]([CH2:11][NH:12][C@H:13]2[CH2:18][CH2:17][C@H:16]([C:19]([CH3:20])([CH3:21])[CH3:22])[CH2:15][CH2:14]2)=[CH:9][CH:10]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 178502669HCID 178502669, 화합물

생성물 1

HCID 178502668HCID 178502668, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

N-Methoxy-N-methyl-trans-4-{[tert-butoxycarbonyl-(4-tert-butylcyclohexyl)amino]methyl}benzamide (1.0 g, 2.3 mmol) was dissolved in DCM (10 ml), and TFA (10 ml) was added. The reaction mixture was stirred at ambient temperature for 2 hours and then taken to dryness by rotary evaporation. The crystal-line residue was then dissolved in ethyl acetate (100 ml), and the organic phase was washed with saturated aqueous sodium carbonate solution (2×100 ml). The combined water phases were back extracted once with ethyl acetate (100 ml); and the combined organic phases dried with anhydrous sodium sulphate. Solvent was removed by rotary evaporation, to leave the title product as fine white crystals. Yield: 760 mg (99%).

후처리

  1. customtaken to dryness by rotary evaporation
  2. dissolutionThe crystal-line residue was then dissolved in ethyl acetate (100 ml)
  3. washthe organic phase was washed with saturated aqueous sodium carbonate solution (2×100 ml)
  4. extractionThe combined water phases were back extracted once with ethyl acetate (100 ml)
  5. dry with materialand the combined organic phases dried with anhydrous sodium sulphate
  6. customSolvent was removed by rotary evaporation

출처 및 근거

ORD 기록
ord-4b6b740607294a6e8585e669c5b49fa5
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06649641B2

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