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Diisopropylethylamine → HCID 86620614, 화합물

HRID 2189913
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HRID 2189913 반응식
[Cl:1][C:2]1[N:9]=[C:8](Cl)[C:7]([Cl:11])=[CH:6][C:3]=1[C:4]#[N:5].[CH3:12][C:13]1[NH:17][N:16]=[C:15]([NH2:18])[CH:14]=1.CCN(C(C)C)C(C)C>CCO>[Cl:1][C:2]1[N:9]=[C:8]([NH:18][C:15]2[CH:14]=[C:13]([CH3:12])[NH:17][N:16]=2)[C:7]([Cl:11])=[CH:6][C:3]=1[C:4]#[N:5]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 931461H-Pyrazol-3-amine, 5-methyl-HCID 229063392,5,6-Trichloronicotinonitrile

생성물 1

HCID 86620614HCID 86620614, 화합물수율 59.8%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
55 °C

실험 절차

To a 25-ml, round-bottom flask, was added 2,5,6-trichloronicotinonitrile (Method 44, 1 g, 4.8 mmol), 5-methyl-1H-pyrazol-3-amine (466 mg, 4.8 mmol), DIEA (1.1 ml, 6.3 mmol), and EtOH (5 ml) and set to heat at 55° C. for 16 hours. The resulting mixture was then purified by silica gel chromatography (Biotage Horizon System) using 25-75% EtOAc/hexanes to give 770 mg of the title compound. 1H NMR: 12.36 (s, 1H) 9.68 (s, 1H) 8.39 (s, 1H) 6.32 (s, 1H) 2.29 (s, 3H). MS: Calcd.: 268. Found: [M+H]+ 267/269.

후처리

  1. customThe resulting mixture was then purified by silica gel chromatography (Biotage Horizon System)

출처 및 근거

ORD 기록
ord-96ffad581d894908b656975596b035c0
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08324252B2

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