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Dicyclohexylcarbodiimide → 2-(6-chloro-5-methylpyridin-3-yl)-N-(5-(pyrazin-2-yl)pyridin-2-yl)acetamide

HRID 592152
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HRID 592152 반응식
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][C:9]([OH:11])=O)=[CH:4][C:3]=1[CH3:12].[N:13]1[CH:18]=[CH:17][N:16]=[CH:15][C:14]=1[C:19]1[CH:20]=[CH:21][C:22]([NH2:25])=[N:23][CH:24]=1.C1(N=C=NC2CCCCC2)CCCCC1>CN(C)C1C=CN=CC=1.CN(C=O)C>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8][C:9]([NH:25][C:22]2[CH:21]=[CH:20][C:19]([C:14]3[CH:15]=[N:16][CH:17]=[CH:18][N:13]=3)=[CH:24][N:23]=2)=[O:11])=[CH:4][C:3]=1[CH3:12]
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참가 물질

6

반응물 3

HCID 10868DicyclohexylcarbodiimideHCID 552673572-(6-Chloro-5-methylpyridin-3-yl)acetic acidHCID 592592255-(Pyrazin-2-yl)pyridin-2-amine

생성물 1

HCID 866579532-(6-chloro-5-methylpyridin-3-yl)-N-(5-(pyrazin-2-yl)pyridin-2-yl)acetamide

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매
HCID 6228
Dimethylformamide
용매

실험 절차

A mixture of 2-(6-chloro-5-methylpyridin-3-yl)acetic acid 86-7 (3.0 g, 16.2 mmol), 5-(pyrazin-2-yl)pyridin-2-amine 86-3 (2.80 g, 16.2 mmol), 1,3-dicyclohexylcarbodiimide (4 g, 19.44 mmol) and 4-(dimethylamino)pyridine (324 mg, 3.24 mmol) in DMF (45 mL) was stirred at room temperature for 10 hours. The reaction mixture was filtered to remove the solid and the filtrate was diluted with ethyl acetate, washed with water and brine, dried over Na2SO4 and concentrated to dryness by rotary evaporation. The crude product was purified by silica gel flash chromatography, eluted with 5% methanol in dichloromethane to give 2-(6-chloro-5-methylpyridin-3-yl)-N-(5-(pyrazin-2-yl)pyridin-2-yl)acetamide 86-8 as pale yellow solid. MS m/z 340.2 (M+1); 1H NMR 400 MHz (DMSO-d6) δ 11.09(s 1H), 9.31(d, 1H, J=1.6 Hz), 9.11(d, 1H, J=1.6 Hz), 8.72(m, 1H), 8.63(m, 1H), 8.51(dd, 1H, J1=8.6 Hz, J2=2.4 Hz), 8.21(m, 2H), 7.76(d, 1H, J=1.6 Hz), 3.82(s, 2H), 2.33(s, 3H).

후처리

  1. filtrationThe reaction mixture was filtered
  2. customto remove the solid
  3. additionthe filtrate was diluted with ethyl acetate
  4. washwashed with water and brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated to dryness by rotary evaporation
  7. customThe crude product was purified by silica gel flash chromatography
  8. washeluted with 5% methanol in dichloromethane

출처 및 근거

ORD 기록
ord-371a41f462d94b36b5508838a6ec9f45
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09238646B2

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