Trifluoroacetic acid → 1-(5-(2-(Piperazin-1-yl)ethyl)indolin-1-yl)ethanone

HRID 535649

反応式

HRID 535649 の反応式
FC(F)(F)C(O)=O.[C:8]([N:11]1[C:19]2[C:14](=[CH:15][C:16]([CH2:20][CH2:21][N:22]3[CH2:27][CH2:26][N:25](C(OC(C)(C)C)=O)[CH2:24][CH2:23]3)=[CH:17][CH:18]=2)[CH2:13][CH2:12]1)(=[O:10])[CH3:9]>C(Cl)Cl>[N:22]1([CH2:21][CH2:20][C:16]2[CH:15]=[C:14]3[C:19](=[CH:18][CH:17]=2)[N:11]([C:8](=[O:10])[CH3:9])[CH2:12][CH2:13]3)[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 59636762Tert-butyl 4-(2-(1-acetylindolin-5-yl)ethyl)piperazine-1-carboxylate

生成物 1

HCID 596367471-(5-(2-(Piperazin-1-yl)ethyl)indolin-1-yl)ethanone収率 101.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoroacetic acid (4.08 mL, 53.08 mmol) was added to a solution of tert-butyl 4-(2-(1-acetylindolin-5-yl)ethyl)piperazine-1-carboxylate (0.793 g, 2.12 mmol) in dry DCM and the reaction was stirred at room temperature for 60 min. The mixture was evaporated and the crude mixture was made basic with 10% NaOH aq. The aq phase was extracted with DCM (3×), dried (Na2SO4), filtered and evaporated to give 0.590 g of the product. This product was taken to the next step assuming quantitative yield without further purification. MS (ES+) m/z 274.2 (M+H)+.

後処理

  1. customThe mixture was evaporated
  2. extractionwas extracted with DCM (3×)
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated

出典と根拠

ORDレコード
ord-385d2204b28b418eb06835bd6ce6981d
出典データセット
uspto-grants-2014_10
特許番号
US08859534B2

関連ノート

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