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Sodium hydride → HCID 178425256, 화합물

HRID 252982
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HRID 252982 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][CH:29]=1)[CH:5]=[N:6][NH:7][C:8]1[CH:13]=[C:12]([N:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)[N:11]=[C:10]([CH2:20][CH2:21]OS(C)(=O)=O)[N:9]=1.[N:30]1[CH:35]=[CH:34][C:33]([C:36]2[NH:37][C:38]([SH:41])=[N:39][N:40]=2)=[CH:32][CH:31]=1.[H-].[Na+]>O1CCCC1>[CH3:1][C:2]1[CH:3]=[C:4]([CH:27]=[CH:28][CH:29]=1)[CH:5]=[N:6][NH:7][C:8]1[CH:13]=[C:12]([N:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)[N:11]=[C:10]([CH2:20][CH2:21][S:41][C:38]2[NH:37][C:36]([C:33]3[CH:34]=[CH:35][N:30]=[CH:31][CH:32]=3)=[N:40][N:39]=2)[N:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 76837803methanesulfonic acid 2-{4-[N'-(3-methyl-benzylidene)-hydrazino]-6-morpholin-4-yl-pyrimidin-2-yl}-ethyl esterHCID 1785279605-pyridin-4-yl-1H-1,2,4-triazole-3-thiol

생성물 1

HCID 178425256HCID 178425256, 화합물수율 56.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Compound 95, methanesulfonic acid 2-{4-[N′-(3-methyl-benzylidene)-hydrazino]-6-morpholin-4-yl-pyrimidin-2-yl}-ethyl ester (50 mg., 0.12 mmol) was dissolved in tetrahydrofuran (2 mL). To the reaction mixture was added 5-pyridin-4-yl-4H-[1,2,4]triazole-3-thiol (124 mg., 0.66 mmol) and sodium hydride (12 mg., 0.5 mmol) and the vessel was stirred at room temperature for sixteen hours. The solvent was removed under reduced pressure and the crude oil was purified by column chromatography to give Compound 25, N-(3-methyl-benzylidene)-N′-{6-morpholin-4-yl-2-[2-(5-pyridin-4-yl-4H-[1,2,4]triazol-3-ylsulfanyl)-ethyl]-pyrimidin-4-yl}-hydrazine (34 mg.).

후처리

  1. customThe solvent was removed under reduced pressure
  2. customthe crude oil was purified by column chromatography

출처 및 근거

ORD 기록
ord-bd8bb426d8a642d68913c686fa05ff47
출처 데이터셋
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07872005B2

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