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Potassium Carbonate → (2,6-Dichloro-3-{[methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amino]-methyl}-pyridin-4-yl)-pyrrolidin-1-yl-methanone

HRID 1392671
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HRID 1392671 반응식
[Cl:1][C:2]1[C:7]([CH2:8]O)=[C:6]([C:10]([N:12]2[CH2:16][CH2:15][CH2:14][CH2:13]2)=[O:11])[CH:5]=[C:4]([Cl:17])[N:3]=1.O=S(Cl)Cl.C([O-])([O-])=O.[K+].[K+].[CH3:28][NH:29][C@@H:30]1[C:39]2[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=2)[CH2:33][CH2:32][CH2:31]1>C(Cl)Cl.O.CCOC(C)=O.CC#N>[Cl:1][C:2]1[C:7]([CH2:8][N:29]([CH3:28])[CH:30]2[C:39]3[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=3)[CH2:33][CH2:32][CH2:31]2)=[C:6]([C:10]([N:12]2[CH2:16][CH2:15][CH2:14][CH2:13]2)=[O:11])[CH:5]=[C:4]([Cl:17])[N:3]=1
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참가 물질

9

반응물 4

HCID 11430Potassium CarbonateHCID 24386Thionyl ChlorideHCID 7128547(1S)-1,2,3,4-Tetrahydro-N-methyl-1-naphthalenamineHCID 59678084(2,6-Dichloro-3-hydroxymethyl-pyridin-4-yl)-pyrrolidin-1-yl-methanone

생성물 1

HCID 72355817(2,6-Dichloro-3-{[methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amino]-methyl}-pyridin-4-yl)-pyrrolidin-1-yl-methanone

시약·촉매·용매 4

HCID 962Water용매HCID 6342Acetonitrile용매HCID 6344Dichloromethane용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of (2,6-dichloro-3-hydroxymethyl-pyridin-4-yl)-pyrrolidin-1-yl-methanone (400 mg, 1.45 mmol) and SOCl2 (1 mL) in CH2Cl2 (10 mL) is stirred at room temperature for 1 hour, and then concentrated. The residue is treated with K2CO3 (1.0 g, 7.2 mmol), CH3CN (10 mL) and (S)-methyl-(1,2,3,4-tetrahydro-naphthalen-1-yl)-amine (250 mg, 1.55 mmol). The resulting mixture is stirred at room temperature overnight. EtOAc (50 mL) and water (40 mL) are added to the residue. The organic layer is separated, washed once with brine, dried (Na2SO4) and concentrated. The residue is chromatographed on silica gel (4:1 hexane:EtOAc) to give the title compound.

후처리

  1. concentrationconcentrated
  2. stirringThe resulting mixture is stirred at room temperature overnight
  3. customThe organic layer is separated
  4. washwashed once with brine
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated
  7. customThe residue is chromatographed on silica gel (4:1 hexane:EtOAc)

출처 및 근거

ORD 기록
ord-b544b6264dce40f6b70173e666811b95
출처 데이터셋
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07342115B2

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