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Sodium hydride → 1-[N-Cyclopropylmethyl-N-(5,6-dimethyl-2-methoxypyridin-3-yl)aminocarbonyl]-4-(2-methoxyphenyl)piperazine

HRID 377910
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HRID 377910 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([NH:11][C:12]([N:14]2[CH2:19][CH2:18][N:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[O:26][CH3:27])[CH2:16][CH2:15]2)=[O:13])[C:5]([O:9][CH3:10])=[N:6][C:7]=1[CH3:8].[H-].[Na+].Br[CH2:31][CH:32]1[CH2:34][CH2:33]1>CN(C)C=O>[CH:32]1([CH2:31][N:11]([C:4]2[C:5]([O:9][CH3:10])=[N:6][C:7]([CH3:8])=[C:2]([CH3:1])[CH:3]=2)[C:12]([N:14]2[CH2:15][CH2:16][N:17]([C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[O:26][CH3:27])[CH2:18][CH2:19]2)=[O:13])[CH2:34][CH2:33]1
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참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 81503BromomethylcyclopropaneHCID 193571181-[(5,6-Dimethyl-2-methoxypyridin-3-yl)aminocarbonyl]-4-(2-methoxyphenyl)piperazine

생성물 1

HCID 193569611-[N-Cyclopropylmethyl-N-(5,6-dimethyl-2-methoxypyridin-3-yl)aminocarbonyl]-4-(2-methoxyphenyl)piperazine수율 78%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

1-[(5,6-Dimethyl-2-methoxypyridin-3-yl)aminocarbonyl]-4-(2-methoxyphenyl)piperazine(100 mg, 0.26 mmol) was dissolved in dimethylformamide(15 ml) and thereto sodium hydride(6.2 mg, 0.26 mmol) was added, followed by stirring at room temperature for 15 min, and successively bromomethylcyclopropane(21.8 mg, 0.26 mmol) was added. The resulting mixture was stirred at room temperature for 16 hrs, concentrated under the reduced pressure and purified by column chromatography(ethylacetate:hexane=1:2) to obtain the titled compound.

후처리

  1. stirringThe resulting mixture was stirred at room temperature for 16 hrs
  2. concentrationconcentrated under the reduced pressure
  3. custompurified by column chromatography(ethylacetate:hexane=1:2)

출처 및 근거

ORD 기록
ord-ce8d7809756446409236b54a2ab8ba83
출처 데이터셋
uspto-grants-2000_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06028195

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