Cesium carbonate → 4-Octylindoline

HRID 710485

反応式

HRID 710485 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 667295994-Octylindoline収率 93%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-05a4f5eea4844221a40bc8ac32ab01a2
出典データセット
uspto-grants-2015_11
特許番号
US09181182B2

関連ノート

読み込み中…