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Triethylamine → 1-(4-Chlorophenyl)-n-(5-methyl-6-(5-methyl-6-oxo-1,6-dihydropyridin-3-yl)pyridin-2-yl)cyclopropanecarboxamide

HRID 870007
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HRID 870007 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:11]([OH:13])=O)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.S(Cl)(Cl)=O.C[O:19][C:20]1[N:25]=[CH:24][C:23]([C:26]2[C:31]([CH3:32])=[CH:30][CH:29]=[C:28]([NH2:33])[N:27]=2)=[CH:22][C:21]=1[CH3:34].C(N(CC)CC)C>ClCCl.CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([C:11]([NH:33][C:28]3[CH:29]=[CH:30][C:31]([CH3:32])=[C:26]([C:23]4[CH:22]=[C:21]([CH3:34])[C:20](=[O:19])[NH:25][CH:24]=4)[N:27]=3)=[O:13])[CH2:9][CH2:10]2)=[CH:6][CH:7]=1
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참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 24386Thionyl ChlorideHCID 986061-(p-Chlorophenyl)cyclopropanecarboxylic acidHCID 68722468HCID 68722468, 화합물

생성물 1

HCID 710530451-(4-Chlorophenyl)-n-(5-methyl-6-(5-methyl-6-oxo-1,6-dihydropyridin-3-yl)pyridin-2-yl)cyclopropanecarboxamide수율 78.7%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
촉매
HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 1-(4-chlorophenyl)cyclopropanecarboxylic acid (39.3 mg, 0.2 mmol) in dichloromethane (2 mL) was added thionyl chloride (43.8 μL, 0.6 mmol) followed by DMF (1 drop) and the reaction was stirred at room temperature for 30 minutes and then the solvent was removed. Toluene (˜1 mL) was added, mixed with the residue and then removed by evaporation. The residue was then dissolved in dichloromethane (1 mL) and a solution of 6′-methoxy-3,5′-dimethyl-2,3′-bipyridin-6-amine (46 mg, 0.2 mmol) and triethyl amine (83.6 μL, 0.60 mmol) in dichloromethane (1 mL) was added. The reaction was stirred at room temperature for 12 hors. The reaction was then concentrated. The residue was dissolved in DMSO and purified by reverse phase HPLC (10-99% acetonitrile/water) to yield 62 mg of the product. ESI-MS m/z calc. 407.1. found 408.2 (M+1)+. Retention time 2.07 minutes.

후처리

  1. customthe solvent was removed
  2. additionToluene (˜1 mL) was added
  3. additionmixed with the residue
  4. customremoved by evaporation
  5. dissolutionThe residue was then dissolved in dichloromethane (1 mL)
  6. stirringThe reaction was stirred at room temperature for 12 hors
  7. concentrationThe reaction was then concentrated
  8. dissolutionThe residue was dissolved in DMSO
  9. custompurified by reverse phase HPLC (10-99% acetonitrile/water)

출처 및 근거

ORD 기록
ord-7c2ae0741bdf4151ad65887395542f20
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969386B2

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