Sodium hydride → 2-Bromo-5-(4-methylpiperazin-1-YL)pyrazine

HRID 1157310노트

반응식

HRID 1157310 반응식
[H-].[Na+].[CH3:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.Br[C:11]1[C:16]([Br:17])=[N:15][CH:14]=[CH:13][N:12]=1>C1COCC1>[Br:17][C:16]1[CH:11]=[N:12][C:13]([N:7]2[CH2:8][CH2:9][N:4]([CH3:3])[CH2:5][CH2:6]2)=[CH:14][N:15]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 531671-MethylpiperazineHCID 138675722,3-Dibromopyrazine

생성물 1

HCID 457877252-Bromo-5-(4-methylpiperazin-1-YL)pyrazine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To sodium hydride (0.20 g) taken in dry THF (15 ml), N-methyl piperazine (0.93 ml) was added under nitrogen at 0° C. 2,3-Dibromopyrazine (2 g) taken in 15 ml dry THF was added to the above mixture at 0° C. The reaction mixture was allowed to reflux for overnight and quenched with water (5 ml). The organic layer was removed under vacuum. The resulting crude mass was purified by column chromatography to afford 2-bromo-5-(4-methylpiperazin-1-yl)pyrazine as pure product.

후처리

  1. additionwas added to the above mixture at 0° C
  2. temperatureto reflux for overnight
  3. customquenched with water (5 ml)
  4. customThe organic layer was removed under vacuum
  5. customThe resulting crude mass was purified by column chromatography

출처 및 근거

ORD 기록
ord-19fe532ae53b45c6ae9611834c4732c5
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07807671B2

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