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Formaldehyde → Diethyl 2-(4-(4-methylpiperazin-1-yl)benzyl)-2-methylmalonate

HRID 1896276
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HRID 1896276 반응식
[N:1]1([C:7]2[CH:25]=[CH:24][C:10]([CH2:11][C:12]([CH3:23])([C:18]([O:20][CH2:21][CH3:22])=[O:19])[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:9][CH:8]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[CH2:26]=O>C(O)=O>[CH3:26][N:4]1[CH2:5][CH2:6][N:1]([C:7]2[CH:8]=[CH:9][C:10]([CH2:11][C:12]([CH3:23])([C:18]([O:20][CH2:21][CH3:22])=[O:19])[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:24][CH:25]=2)[CH2:2][CH2:3]1
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참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 67382829Diethyl 2-(4-(piperazin-1-yl)benzyl)-2-methylmalonate

생성물 1

HCID 67383064Diethyl 2-(4-(4-methylpiperazin-1-yl)benzyl)-2-methylmalonate수율 86.8%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

A mixture of diethyl 2-(4-(piperazin-1-yl)benzyl)-2-methylmalonate (500 mg, 1.43 mmol), formaldehyde (2 ml) and formic acid (2 ml) was heated at reflux for 2 h. The reaction mixture was concentrated and partitioned between saturated sodium bicarbonate solution and ethyl acetate. The organic layer was separated and washed with water, brine solution, dried over anhydrous sodium sulfate, filtered and concentrated to afford 400 mg (86.8%) of diethyl 2-(4-(4-methylpiperazin-1-yl)benzyl)-2-methylmalonate as brown oil.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2 h
  3. concentrationThe reaction mixture was concentrated
  4. custompartitioned between saturated sodium bicarbonate solution and ethyl acetate
  5. customThe organic layer was separated
  6. washwashed with water, brine solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-90221e893cc242e2a15b901090866b29
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08518948B2

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