Sodium Carbonate → 3-Iodo-2-methyl-5-nitropyridine

HRID 77731노트

반응식

HRID 77731 반응식
[I:1][C:2]1[C:3]([CH:11](C(OCC)=O)C(OCC)=O)=[N:4][CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1.C([O-])([O-])=O.[Na+].[Na+]>S(=O)(=O)(O)O>[I:1][C:2]1[C:3]([CH3:11])=[N:4][CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1

참가 물질

4

반응물 2

HCID 10340Sodium CarbonateHCID 59776929Diethyl (3-iodo-5-nitropyridin-2-yl)malonate

생성물 1

HCID 591983253-Iodo-2-methyl-5-nitropyridine

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

Diethyl (3-iodo-5-nitropyridin-2-yl)malonate (0.250 g, 0.000612 mol) was heated in 6 M sulfuric acid (3 mL) at 100° C. for 16 hours. The reaction was neutralized with solid Na2CO3, extracted with EtOAc and the organic extracts were washed with water, saturated NaCl, dried (MgSO4) and stripped in vacuo. NMR analysis indicated that it was clean enough for the next reaction. 1H NMR (400 MHZ, CDCl3): δ 9.27 (d, 1H), 8.82 (d, 1H), 2.87 (s, 3H); MS (ES) (M+H)=265.

후처리

  1. extractionextracted with EtOAc
  2. washthe organic extracts were washed with water, saturated NaCl
  3. dry with materialdried (MgSO4)
  4. customwas clean enough for the next reaction

출처 및 근거

ORD 기록
ord-b2b834e8ae7f449d8368a7933a6f338c
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841318B2

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