2-Dimethylaminopyridine → HCID 14304997, 화합물

HRID 477057노트

반응식

HRID 477057 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH2:17])[CH2:9][CH2:8]1.[O:18]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[C:21](=[O:22])[C:20]([C:29](O)=[O:30])=[C:19]1[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1.CN(C1C=CC=CN=1)C.CS(Cl)(=O)=O>ClCCl>[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[N:7]1[CH2:8][CH2:9][N:10]([CH2:13][CH2:14][CH2:15][CH2:16][NH:17][C:29]([C:20]2[C:21](=[O:22])[C:23]3[C:28](=[CH:27][CH:26]=[CH:25][CH:24]=3)[O:18][C:19]=2[C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)=[O:30])[CH2:11][CH2:12]1

참가 물질

6

반응물 4

HCID 218852-DimethylaminopyridineHCID 31297Methanesulfonyl chlorideHCID 12674946HCID 12674946, 화합물HCID 14295622HCID 14295622, 화합물

생성물 1

HCID 14304997HCID 14304997, 화합물수율 64.8%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

3.6 g of the 4-[4-(2-pyridyl)-piperazin-1-yl]butylamine obtained above were added to a reaction mixture cooled to -2020 C. which contained, in 100 ml of absolute dichloromethane, a mixed anhydride produced in a manner analogous to Example 1 (a) from 4.0 g flavone-3-carboxylic acid, 3.367 g dimethylaminopyridine and 1.28 ml methanesulfonyl chloride. The reaction mixture was allowed to warm up to room temperature and stirred at room temperature for two hours. Subsequently the reaction mixture was worked up analogously to Example 3, and the resulting title compound was recrystallized from ethylacetate. There were obtained 4.7 g 3-{4-[4-(2-pyridyl)-piperazin-1-yl]-butylaminocarbonyl}flavone.

후처리

  1. additionabove were added to a reaction mixture
  2. temperaturecooled to -2020 C
  3. customthe resulting title compound was recrystallized from ethylacetate

출처 및 근거

ORD 기록
ord-9ada4ac23ead42588bc52fa437a22f17
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04886806

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