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2-Chloro-5-nitrobenzonitrile → 1,3-dimethyl-6-{4-[3-(2-cyano-4-nitroanilino)propyl]piperazin-1-yl}-2,4(1H,3H)-pyrimidinedione

HRID 1085277
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HRID 1085277 반응식
[CH3:1][N:2]1[C:7]([N:8]2[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][CH2:16][N:17](S(CC)(=O)=O)[C:18]3[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][CH:19]=3)[CH2:10][CH2:9]2)=[CH:6][C:5](=[O:32])[N:4]([CH3:33])[C:3]1=[O:34].ClC1C=CC([N+]([O-])=O)=CC=1[C:38]#[N:39]>CN(C)C=O>[CH3:1][N:2]1[C:7]([N:8]2[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][CH2:16][NH:17][C:18]3[CH:19]=[CH:20][C:21]([N+:24]([O-:26])=[O:25])=[CH:22][C:23]=3[C:38]#[N:39])[CH2:12][CH2:13]2)=[CH:6][C:5](=[O:32])[N:4]([CH3:33])[C:3]1=[O:34]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 855042-Chloro-5-nitrobenzonitrileHCID 200610721,3-dimethyl-6-{4-[3-(N-ethanesulfonyl-4-nitroanilino)propyl]piperazin-1-yl}-2,4(1H,3H)-pyrimidinedione

생성물 1

HCID 200611961,3-dimethyl-6-{4-[3-(2-cyano-4-nitroanilino)propyl]piperazin-1-yl}-2,4(1H,3H)-pyrimidinedione수율 154.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

0.3 g of Compound 158 obtained beforehand, 0.3 g of 2-chloro-5-nitrobenzonitrile and 0.31 ml of trtiethylamine were stirred at 80° C. for 1 hour in 5 ml of dimethylformamide. The reaction mixture was concentrated under reduced pressure and the residue was purified by chromatography on a silica gel column (eluent: chloroform/methanol=40/1, by volume), thereby obtaining 0.4 g of 1,3-dimethyl-6-{4-[3-(2-cyano-4-nitroanilino)propyl]piperazin-1-yl}-2,4(1H,3H)-pyrimidinedione.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was purified by chromatography on a silica gel column (eluent: chloroform/methanol=40/1, by volume)

출처 및 근거

ORD 기록
ord-df36c8d6c9f04c058a8b35314c43a1ef
출처 데이터셋
uspto-grants-1991_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05008267

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