Sodium hydride → 4-Cyclopropylmethoxy-2-methylpyridine-1-oxide

HRID 327776

反応式

HRID 327776 の反応式
[H-].[Na+].[CH3:3][C:4]1[CH:9]=[C:8]([N+]([O-])=O)[CH:7]=[CH:6][N+:5]=1[O-:13].[CH:14]1([CH2:17][OH:18])[CH2:16][CH2:15]1>>[CH:14]1([CH2:17][O:18][C:8]2[CH:7]=[CH:6][N+:5]([O-:13])=[C:4]([CH3:3])[CH:9]=2)[CH2:16][CH2:15]1

参加物

4

反応物 3

HCID 24758Sodium hydrideHCID 75644Cyclopropanemethanol2 回HCID 95291Pyridine, 2-methyl-4-nitro-, 1-oxide

生成物 1

HCID 107024944-Cyclopropylmethoxy-2-methylpyridine-1-oxide

反応条件

温度
90 °C

実験手順

To sodium hydride (55% pure) (4.4 g, 0.1 mol) (washed with petroleum ether), cyclopropyl-methanol (50 ml) was added. Then a solution of 2-methyl-4-nitropyridine-N-oxide (6.5 g, 0.042 mol) in cyclopropylmethanol (30 ml) was added during about 1 h. The dark brown mixture was heated to 90° C. and stirred at 90° C. for about 1 h. Thereafter the cyclopropylmethanol was distilled off under reduced pressure and methylene chloride (100 ml) was added to the residue. The mixture was stirred for about 30 minutes, then filtered and concentrated which gave 9.5 g of crude material.

後処理

  1. distillationThereafter the cyclopropylmethanol was distilled off under reduced pressure and methylene chloride (100 ml)
  2. additionwas added to the residue
  3. stirringThe mixture was stirred for about 30 minutes
  4. filtrationfiltered
  5. concentrationconcentrated which

出典と根拠

ORDレコード
ord-73e7c7723bfe43eea292efd9bcfc5902
出典データセット
uspto-grants-1993_12
特許番号
US05274099

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