1-(3-Aminopropyl)-4-methylpiperazine → 2-{5-Methyl-2-[3-(4-methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophene-6-carboxylic acid methyl ester

HRID 1986187

반응식

HRID 1986187 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[CH:12]=[C:11]([C:13]3[C:18]([CH3:19])=[CH:17][N:16]=[C:15](Cl)[N:14]=3)[S:10][C:9]=2[CH:21]=1)=[O:4].[NH2:22][CH2:23][CH2:24][CH2:25][N:26]1[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]1>O1CCOCC1>[CH3:1][O:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]2[CH:12]=[C:11]([C:13]3[C:18]([CH3:19])=[CH:17][N:16]=[C:15]([NH:22][CH2:23][CH2:24][CH2:25][N:26]4[CH2:27][CH2:28][N:29]([CH3:32])[CH2:30][CH2:31]4)[N:14]=3)[S:10][C:9]=2[CH:21]=1)=[O:4]

참가 물질

4

반응물 2

HCID 783281-(3-Aminopropyl)-4-methylpiperazineHCID 866253462-(2-Chloro-5-methylpyrimidin-4-yl)-benzo[b]thiophene-6-carboxylic acid methyl ester

생성물 1

HCID 688570602-{5-Methyl-2-[3-(4-methylpiperazin-1-yl)-propylamino]-pyrimidin-4-yl}-benzo[b]thiophene-6-carboxylic acid methyl ester수율 72%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
90 °C

실험 절차

A mixture of 2-(2-chloro-5-methylpyrimidin-4-yl)-benzo[b]thiophene-6-carboxylic acid methyl ester (2.08 g, 6.50 mmol) and 1-(3-aminopropyl)-4-methylpiperazine (3.00 g, 19.0 mmol) in 1,4-dioxane (40 mL) is heated at 90° C. for 20 hours. The solvent is evaporated and the resulting residue is subjected to chromatography on silica gel, eluting with 2M NH3/CH3OH in dichloromethane 0-8%, to give the title compound (1.30 g, 72% yield). ES+(m/z) 460 [M+H].

후처리

  1. customThe solvent is evaporated
  2. washeluting with 2M NH3/CH3OH in dichloromethane 0-8%

출처 및 근거

ORD 기록
ord-8a9f96bbd87b4881b66fd75a0abe2df2
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07547691B2

연결된 노트

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