1,4'-Bipiperidine → 1,3-Dimethyl-7-[4-[6-(4-piperidinopiperidino)-nicotinoyl]benzyl]xanthine

HRID 1291419노트

반응식

HRID 1291419 반응식
Cl[C:2]1[CH:29]=[CH:28][C:5]([C:6]([C:8]2[CH:27]=[CH:26][C:11]([CH2:12][N:13]3[C:21]4[C:20](=[O:22])[N:19]([CH3:23])[C:18](=[O:24])[N:17]([CH3:25])[C:16]=4[N:15]=[CH:14]3)=[CH:10][CH:9]=2)=[O:7])=[CH:4][N:3]=1.[N:30]1([CH:36]2[CH2:41][CH2:40][NH:39][CH2:38][CH2:37]2)[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1>N1C=CC=CC=1.O>[CH3:23][N:19]1[C:20](=[O:22])[C:21]2[N:13]([CH2:12][C:11]3[CH:26]=[CH:27][C:8]([C:6](=[O:7])[C:5]4[CH:28]=[CH:29][C:2]([N:39]5[CH2:40][CH2:41][CH:36]([N:30]6[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]6)[CH2:37][CH2:38]5)=[N:3][CH:4]=4)=[CH:9][CH:10]=3)[CH:14]=[N:15][C:16]=2[N:17]([CH3:25])[C:18]1=[O:24]

참가 물질

5

반응물 2

HCID 786071,4'-BipiperidineHCID 189188457-[4-(6-Chloronicotinoyl)benzyl]-1,3-dimethylxanthine

생성물 1

HCID 189190251,3-Dimethyl-7-[4-[6-(4-piperidinopiperidino)-nicotinoyl]benzyl]xanthine수율 41.7%

시약·촉매·용매 2

HCID 962Water용매HCID 1049Pyridine용매

실험 절차

A solution of 7-[4-(6-chloronicotinoyl)benzyl]-1,3-dimethylxanthine (196 mg) and 4-piperidinopiperidine (102 mg) in pyridine (10 ml) was stirred at 60° C. for 5 hours. This reaction mixture was poured in water and extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The residue was purified by silica gel column chromatography (ethyl acetate: acetone: triethylamine 1:1:0.1) to provide the title compound (108 mg).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate: acetone: triethylamine 1:1:0.1)

출처 및 근거

ORD 기록
ord-86f3f315b9044a4db53fbcd9e1a2322b
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753664

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