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

HRID 77731ノート

反応式

HRID 77731 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b2b834e8ae7f449d8368a7933a6f338c
出典データセット
uspto-grants-2014_09
特許番号
US08841318B2

反応ノート

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