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

HRID 327776

반응식

HRID 327776 반응식
[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

참가 물질

4

반응물 3

HCID 24758Sodium hydrideHCID 75644Cyclopropanemethanol2회HCID 95291Pyridine, 2-methyl-4-nitro-, 1-oxide

생성물 1

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

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-73e7c7723bfe43eea292efd9bcfc5902
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05274099

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