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Sodium Carbonate → 4-tert-butyl-2,3-dimethylpyridine N-oxide

HRID 35458
ノート
印刷プレビュー

反応式

HRID 35458 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][N:8]=[C:7]([CH3:11])[C:6]=1[CH3:12])([CH3:4])([CH3:3])[CH3:2].ClC1C=CC=C(C(OO)=[O:21])C=1.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)Cl>[C:1]([C:5]1[CH:10]=[CH:9][N+:8]([O-:21])=[C:7]([CH3:11])[C:6]=1[CH3:12])([CH3:4])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 21296013HCID 21296013、化合物

生成物 1

HCID 536584744-tert-butyl-2,3-dimethylpyridine N-oxide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 10.5 g of 4-tert-butyl-2,3-dimethylpyridine in 120 ml of methylene chloride is treated at room temperature with 14.4 g of m-chloroperbenzoic acid. The reaction mixture is made basic with a saturated sodium carbonate solution and extracted. The organic solution is dried and concentrated. The residue is purified on a silica qel column, whereby the medium pressure flash chromatography method (solvent: methylene chloride/ethyl acetate, with increasing ethyl acetate concentrations) is used and the pressure is produced with nitrogen gas. The 4-tert-butyl-2,3-dimethylpyridine N-oxide obtained is processed directly.

後処理

  1. extractionextracted
  2. customThe organic solution is dried
  3. concentrationconcentrated
  4. customThe residue is purified on a silica qel column, whereby
  5. concentrationthe medium pressure flash chromatography method (solvent: methylene chloride/ethyl acetate, with increasing ethyl acetate concentrations)
  6. customthe pressure is produced with nitrogen gas

出典と根拠

ORDレコード
ord-6c291d75f2e4481582b06b95df14ca72
出典データセット
uspto-grants-1988_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04766133

反応ノート

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