Potassium Carbonate → Methyl 2-((5-methoxy-6-nitropyridin-2-yl)methylthio)acetate

HRID 72660

반응식

HRID 72660 반응식
Br[CH2:2][C:3]1[N:8]=[C:7]([N+:9]([O-:11])=[O:10])[C:6]([O:12][CH3:13])=[CH:5][CH:4]=1.C[CH:15]([SH:19])[C:16]([O-:18])=[O:17].[C:20](=O)([O-])[O-].[K+].[K+]>CO>[CH3:13][O:12][C:6]1[CH:5]=[CH:4][C:3]([CH2:2][S:19][CH2:15][C:16]([O:18][CH3:20])=[O:17])=[N:8][C:7]=1[N+:9]([O-:11])=[O:10]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 144051243-Methoxy-2-nitro-6-pyridylmethyl bromideHCID 156077362-Mercaptopropionate

생성물 1

HCID 67994824Methyl 2-((5-methoxy-6-nitropyridin-2-yl)methylthio)acetate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 6-(bromomethyl)-3-methoxy-2-nitropyridine (30 mmol, 0.74 g), methythioglycolate (2.7 mL, 30 mmol), and potassium carbonate (5.5 g, 40 mmol) in methanol (200 mL) was stirred at room temperature for 10 hours. After concentrated the mixture was purified by column chromatography using PE/DCM (1:1, v/v) followed by DCM to the titled compound. 1H-NMR (CDCl3): δ 3.27 (S, 2H, CH2), 3.74 (S, 3H, OCH3), 3.93 (S, 2H, CH2), 3.99 (S, 3H, OCH3), 7.51 (d, 1H, J=8.6 Hz, Py-H), 7.65 (d, 1H, J=8.6 Hz, Py-H); HR-MS (ESI+) m/z 272.0467 [M+H]+ C10H12N2O5S requires 273.0547.

후처리

  1. concentrationAfter concentrated the mixture
  2. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-41f55f15631d41559d11993553177430
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08829003B2

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