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Acetyl chloride → 4-Chloro-2-methyl-1-oxo-1lambda~5~-pyridine

HRID 31681
ノート
印刷プレビュー

反応式

HRID 31681 の反応式
[N+]([C:4]1[CH:5]=[C:6]([CH3:11])[N+:7]([O-:10])=[CH:8][CH:9]=1)([O-])=O.C([Cl:15])(=O)C>C(OCC)(=O)C.C(Cl)(Cl)Cl>[Cl:15][C:4]1[CH:9]=[CH:8][N+:7]([O-:10])=[C:6]([CH3:11])[CH:5]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 6367Acetyl chlorideHCID 95291Pyridine, 2-methyl-4-nitro-, 1-oxide

生成物 1

HCID 122118014-Chloro-2-methyl-1-oxo-1lambda~5~-pyridine収率 16.8%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
-12.5 °C

実験手順

4-nitro-2-picoline N-oxide (20 g, 130 mmol) was added to acetyl chloride (120 ml, 1688 mmol) in a nitrogen atmosphere at −25° C. The mixture was stirred at −30 to 5° C. for 4 hours and 15 minutes. After the reaction mixture was diluted with ethyl acetate (about 150 ml) and chloroform (about 100 ml), the mixture was concentrated. The residue was purified by silica gel column chromatography (NH silica gel: 200 g, elution solvent: heptane, heptane/ethyl acetate=75/25, 50/50, 25/75, ethyl acetate, ethyl acetate/methanol=20/1) to obtain the title compound (3.14 g) as brown oil. Simultaneously, a crude product (about 17 g) was obtained. The crude product thus obtained was further purified by silica gel column chromatography (NH silica gel: 300 g, elution solvent: heptane, heptane/ethyl acetate=75/25, 40/60, 25/75, ethyl acetate) to obtain the title compound (5.39 g) separately as brown oil.

後処理

  1. concentrationthe mixture was concentrated
  2. customThe residue was purified by silica gel column chromatography (NH silica gel: 200 g, elution solvent: heptane, heptane/ethyl acetate=75/25, 50/50, 25/75, ethyl acetate, ethyl acetate/methanol=20/1)

出典と根拠

ORDレコード
ord-b6af840770b1403392ee2ad5c1194c43
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07425634B2

反応ノート

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