Trifluoroacetic acid → 3-(2-Oxo-2-(piperazin-1-yl)ethoxy)benzaldehyde

HRID 592076ノート

反応式

HRID 592076 の反応式
[CH:1]([C:3]1[CH:4]=[C:5]([CH:23]=[CH:24][CH:25]=1)[O:6][CH2:7][C:8]([N:10]1[CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12][CH2:11]1)=[O:9])=[O:2].C(O)(C(F)(F)F)=O>C(Cl)Cl>[O:9]=[C:8]([N:10]1[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]1)[CH2:7][O:6][C:5]1[CH:4]=[C:3]([CH:25]=[CH:24][CH:23]=1)[CH:1]=[O:2]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 89725867Tert-Butyl 4-(2-(3-formylphenoxy)acetyl)piperazine-1-carboxylate2 回

生成物 1

HCID 897262023-(2-Oxo-2-(piperazin-1-yl)ethoxy)benzaldehyde

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

tert-butyl 4-(2-(3-formylphenoxy)acetyl)piperazine-1-carboxylate (49)/(5.55 mmol) was taken in DCM and cooled to 0° C. when TFA (5 ml) was added drop wise and then stirred at rt for 16 h when TLC confirmed completion of reaction. The reaction mixture was concentrated and neutralized with satd NaHCO3 solution followed by extraction with DCM. The combined organic extracts was dried, concentrated and used directly for the next step (86%). LCMS: 98.12% (M++1).

後処理

  1. additionwas added drop wise
  2. customcompletion of reaction
  3. concentrationThe reaction mixture was concentrated
  4. extractionfollowed by extraction with DCM
  5. customThe combined organic extracts was dried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-c18d9be70abe4cc89c3413b3ee5ddc00
出典データセット
uspto-grants-2016_01
特許番号
US09238656B2

反応ノート

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