Water → HCID 60631682、化合物

HRID 1896014ノート

反応式

HRID 1896014 の反応式
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[N:11]1[CH:16]=[CH:15][C:14]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+].O>C(O)CCC>[N+:8]([C:7]1[C:2]([N:11]2[CH2:16][CH2:15][CH:14]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH2:13][CH2:12]2)=[N:3][CH:4]=[CH:5][CH:6]=1)([O-:10])=[O:9]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 15291Ethyl isonicotinateHCID 796132-Chloro-3-nitropyridine

生成物 1

HCID 60631682HCID 60631682、化合物収率 78.3%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A mixture of 2-chloro-3-nitropyridine (1 g, 6.31 mmol), ethyl 4-pyridinecarboxylate (1.19 g, 7.57 mmol) and potassium carbonate (1.31 g, 9.47 mmol) in n-butanol (25 mL) was stirred at reflux for 2 hours, cooled to r.t., poured into water and extracted with diethyl ether. The combined organic layers were washed with brine, dried on Na2SO4 and evaporated to dryness in vacuo to afford a residue, which was purified by flash chromatography (EtOAc—Petroleum Ether 2:8) affording the title product (1.38 g).

後処理

  1. temperatureat reflux for 2 hours
  2. extractionextracted with diethyl ether
  3. washThe combined organic layers were washed with brine
  4. customdried on Na2SO4
  5. customevaporated to dryness in vacuo
  6. customto afford a residue, which
  7. customwas purified by flash chromatography (EtOAc—Petroleum Ether 2:8)

出典と根拠

ORDレコード
ord-4e7abe765fcc4c4f8c442198e4f3898a
出典データセット
uspto-grants-2013_08
特許番号
US08518916B2

反応ノート

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