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

HRID 592076노트

반응식

HRID 592076 반응식
[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]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 89725867Tert-Butyl 4-(2-(3-formylphenoxy)acetyl)piperazine-1-carboxylate2회

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c18d9be70abe4cc89c3413b3ee5ddc00
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09238656B2

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