Cesium carbonate → 4-Octylindoline

HRID 710485

반응식

HRID 710485 반응식
FC(F)(F)C([N:5]1[C:13]2[C:8](=[C:9]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH:10]=[CH:11][CH:12]=2)[CH2:7][CH2:6]1)=O.C([O-])([O-])=O.[Cs+].[Cs+]>CO>[CH2:14]([C:9]1[CH:10]=[CH:11][CH:12]=[C:13]2[C:8]=1[CH2:7][CH2:6][NH:5]2)[CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH3:21]

참가 물질

4

반응물 2

HCID 10796Cesium carbonateHCID 866618152,2,2-Trifluoro-1-(4-octylindolin-1-yl)ethanone

생성물 1

HCID 667295994-Octylindoline수율 93%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of the product of Step C (0.07 g; 0.21 mmol) and Cs2CO3 (0.07 g; 0.21 mmol) in MeOH (2 ml) was stirred overnight at room temperature under N2. After removing solvent under reduced pressure, the residue was diluted to 15 ml with Et2O, washed with H2O, brine, dried over anhydrous MgSO4, filtered and filtrate evaporated to dryness to give the title compound (0.045 g; 93%), as brownish oil, which was used in the next step without further purification. 1H-NMR (CDCl3) 0.86 (m, 3H); 1.28 (m, 10H); 2.47 (m, 2H); 2.95 (m, 2H); 3.52 (m, 2H); 3.7 (broad s, 1H); 6.47-6.54 (m, 2H); 6.89-7.02 (m, 1H).

후처리

  1. customAfter removing solvent under reduced pressure
  2. additionthe residue was diluted to 15 ml with Et2O
  3. washwashed with H2O, brine
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. customfiltrate evaporated to dryness

출처 및 근거

ORD 기록
ord-05a4f5eea4844221a40bc8ac32ab01a2
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09181182B2

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