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

HRID 1894903ノート

反応式

HRID 1894903 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-4b59f538ac634e65aa04009d77fb506f
出典データセット
uspto-grants-2013_08
特許番号
US08513270B2

反応ノート

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