Sodium hydride → Ethyl 2-(4-nitro-1H-imidazole-1-yl)octanoate

HRID 375112

反応式

HRID 375112 の反応式
[N+:1]([C:4]1[N:5]=[CH:6][NH:7][CH:8]=1)([O-:3])=[O:2].[H-].[Na+].Br[CH:12]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[C:13]([O:15][CH2:16][CH3:17])=[O:14]>CN(C=O)C>[N+:1]([C:4]1[N:5]=[CH:6][N:7]([CH:12]([CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:8]=1)([O-:3])=[O:2]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 95580Ethyl 2-bromooctanoateHCID 178526856HCID 178526856、化合物

生成物 1

HCID 10062368Ethyl 2-(4-nitro-1H-imidazole-1-yl)octanoate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4-Nitroimidazole (0.29 moles, 32.9 g in 30 ml DMF was treated portionwise with sodium hydride (0.29 moles, 11.6 g. 60% in mineral oil) and stirred for 45 minutes. Ethyl 2-bromooctanoate (0.29 moles, 73.1 g) was added dropwise over 1 hour. The reaction was stirred overnight at room temperature, poured onto ice water, and extracted with ethyl acetate. The organic phase was washed with brine, dried and concentrated to yield 91 g of ethyl 2-(4-nitro-1H-imidazol-1-yl)octanoate. (MS)

後処理

  1. stirringThe reaction was stirred overnight at room temperature
  2. additionpoured onto ice water
  3. extractionextracted with ethyl acetate
  4. washThe organic phase was washed with brine
  5. customdried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-dbd66e6369174d8aa63f577dbde71f8d
出典データセット
uspto-grants-1996_01
特許番号
US05484780

関連ノート

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