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Formaldehyde → Diethyl 2-methyl-2-(4-(4-methylpiperazin-1-yl)phenyl)malonate

HRID 1896271
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HRID 1896271 반응식
[CH2:1]=O.[CH3:3][C:4]([C:15]1[CH:20]=[CH:19][C:18]([N:21]2[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]2)=[CH:17][CH:16]=1)([C:10]([O:12][CH2:13][CH3:14])=[O:11])[C:5]([O:7][CH2:8][CH3:9])=[O:6]>C(O)=O>[CH3:3][C:4]([C:15]1[CH:20]=[CH:19][C:18]([N:21]2[CH2:22][CH2:23][N:24]([CH3:1])[CH2:25][CH2:26]2)=[CH:17][CH:16]=1)([C:5]([O:7][CH2:8][CH3:9])=[O:6])[C:10]([O:12][CH2:13][CH3:14])=[O:11]
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참가 물질

4

반응물 2

HCID 712FormaldehydeHCID 67382666Diethyl 2-methyl-2-(4-(piperazin-1-yl)phenyl)malonate

생성물 1

HCID 67382777Diethyl 2-methyl-2-(4-(4-methylpiperazin-1-yl)phenyl)malonate수율 70%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

A mixture of formaldehyde (2 ml), formic acid (2 ml) and diethyl 2-methyl-2-(4-(piperazin-1-yl)phenyl)malonate (4.80 g, 14.4 mmol) was heated at reflux for 2 h and the reaction mixture was concentrated under reduced pressure. Saturated sodium bicarbonate solution was added and extracted with ethyl acetate. The organic layer was washed with water, brine solution, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to afford 3.50 g (70.0%) of diethyl 2-methyl-2-(4-(4-methylpiperazin-1-yl)phenyl)malonate as brown oily liquid.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 2 h
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. additionSaturated sodium bicarbonate solution was added
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with water, brine solution
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-fc847cf7d02e456f819bf2e5dac4f3a9
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08518948B2

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