1-(5-Nitropyridin-2-yl)piperazine → HCID 25004371, 화합물

HRID 251424

반응식

HRID 251424 반응식
Cl[C:2]1[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:5]=[C:4]([C:12]2[CH:13]=[C:14]([S:18]([NH2:21])(=[O:20])=[O:19])[CH:15]=[CH:16][CH:17]=2)[C:3]=1[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.[N+:28]([C:31]1[CH:32]=[CH:33][C:34]([N:37]2[CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)=[N:35][CH:36]=1)([O-:30])=[O:29]>N1C=CC=CC=1>[N+:28]([C:31]1[CH:32]=[CH:33][C:34]([N:37]2[CH2:38][CH2:39][N:40]([C:2]3[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:5]=[C:4]([C:12]4[CH:13]=[C:14]([S:18]([NH2:21])(=[O:20])=[O:19])[CH:15]=[CH:16][CH:17]=4)[C:3]=3[C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[CH2:41][CH2:42]2)=[N:35][CH:36]=1)([O-:30])=[O:29]

참가 물질

4

반응물 2

HCID 29287991-(5-Nitropyridin-2-yl)piperazineHCID 866136213-[6-Chloro-5-phenyl-2-(trifluoromethyl)pyrimidin-4-yl]benzenesulfonamide

생성물 1

HCID 25004371HCID 25004371, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

The solution of 3-[6-chloro-5-phenyl-2-(trifluoromethyl)pyrimidin-4-yl]benzenesulfonamide (0.1 g, 0.242 mmol) in pyridine (2 ml) was treated with 1-(5-nitropyridin-2-yl)piperazine (0.075 g, 0.363 mmol) and stirred for 11 hours. Subsequently the reaction mixture was poured onto ice-cold water and extracted with ethyl acetate (25 ml). The organic layer was washed with brine and evaporated to give the crude material. Purification by column chromatography (elution with 70% ethyl acetate in hexane) yielded the title compound. 1H-NMR (CDCl3) δ: 3.45-3.46 (m, 4H), 3.72 (m, 4H), 6.52-6.54 (d, 1H), 7.08-7.11 (d, 2H), 7.21-7.26 (m, 2H), 7.32-7.34 (d, 1H), 7.40-7.42 (d, 1H), 7.50 (m, 1H), 7.68 (s, 1H), 7.84-7.89 (m, 1H), 8.21-8.23 (d, 1H), 8.99 (s, 1H). MS m/z: 585.8 (M+).

후처리

  1. additionSubsequently the reaction mixture was poured onto ice-cold water
  2. extractionextracted with ethyl acetate (25 ml)
  3. washThe organic layer was washed with brine
  4. customevaporated
  5. customto give the crude material
  6. customPurification
  7. washby column chromatography (elution with 70% ethyl acetate in hexane)

출처 및 근거

ORD 기록
ord-e4b6ec0f462f431f916060127fbc5b9b
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07863446B2

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