Dimethyl Sulfoxide → 3-(4-(4-Methylpiperazin-1-yl)phenyl)butanenitrile

HRID 1896281노트

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HRID 1896281 반응식
[C:1]([CH:3]([CH:8]([C:10]1[CH:15]=[CH:14][C:13]([N:16]2[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]2)=[CH:12][CH:11]=1)[CH3:9])C(OC)=O)#[N:2].[Cl-].[Na+].CS(C)=O>O>[CH3:22][N:19]1[CH2:20][CH2:21][N:16]([C:13]2[CH:14]=[CH:15][C:10]([CH:8]([CH3:9])[CH2:3][C:1]#[N:2])=[CH:11][CH:12]=2)[CH2:17][CH2:18]1

참가 물질

5

반응물 3

HCID 679Dimethyl SulfoxideHCID 5234Sodium ChlorideHCID 67382550Methyl 2-cyano-3-(4-(4-methylpiperazin-1-yl)phenyl)butanoate

생성물 1

HCID 673833103-(4-(4-Methylpiperazin-1-yl)phenyl)butanenitrile수율 79.7%

시약·촉매·용매 1

HCID 962Water용매2회

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온도
162.5 °C

실험 절차

A mixture of methyl 2-cyano-3-(4-(4-methylpiperazin-1-yl)phenyl)butanoate (700 mg, 2.32 mmol), sodium chloride (405 mg, 6.90 mmol), DMSO (5 ml) and water (2 ml, 3 vol %) and heated at 160-165° C. for 12 h. The reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water, brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo to afford 450 mg (79.6%) of 3-(4-(4-methylpiperazin-1-yl)phenyl)butanenitrile as a colorless liquid.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water, brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-94792f34f16a4be9b42e843a48acf1f4
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518948B2

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