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Potassium Carbonate → 4-(4-Benzylpiperazin-1-yl)-2-chloropyrimidine

HRID 1699276
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인쇄 미리보기

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HRID 1699276 반응식
[Cl:1][C:2]1[N:7]=[C:6](Cl)[CH:5]=[CH:4][N:3]=1.[C:9]1([CH2:15][N:16]2[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]2)[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+]>O>[Cl:1][C:2]1[N:7]=[C:6]([N:19]2[CH2:20][CH2:21][N:16]([CH2:15][C:9]3[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH2:17][CH2:18]2)[CH:5]=[CH:4][N:3]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 759941-BenzylpiperazineHCID 775312,4-Dichloropyrimidine

생성물 1

HCID 183213004-(4-Benzylpiperazin-1-yl)-2-chloropyrimidine

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
40 °C

실험 절차

A mixture of 9.9 g (0.0664 mol) of 2,4-dichloropyrimidine, 200 ml of water and 11.7 ml (0.0673 mol) of 1-(phenylmethyl)piperazine was heated to 40° C. for 2 hours in an ultrasound bath. After cooling the mixture was made alkaline with potassium carbonate and extracted thoroughly with ethyl acetate. The crude product obtained after working up in the usual way was purified by column chromatography over silica gel (30-60 μm) using FM2 and FM4 (2/1 v/v) as eluant. Working up the appropriate fractions yielded 7.4 g (38.6% of theory) of a colourless oil, Rf=0.51 (FM4; Macherey-Nagel POLYGRAMO® SIL G/UV254, ready-made films for TLC).

후처리

  1. temperatureAfter cooling the mixture
  2. extractionextracted thoroughly with ethyl acetate

출처 및 근거

ORD 기록
ord-3094a39b643b4659903f62eb716630be
출처 데이터셋
uspto-grants-2002_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06344449B1

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