Nitromethane → HCID 66692011、化合物

HRID 2041108ノート

反応式

HRID 2041108 の反応式
[F:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[CH:4]=O.[N+:12]([CH3:15])([O-:14])=[O:13].C([O-])(=O)C.[NH4+]>C(O)(=O)C>[F:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[CH:6][C:3]=1[CH:4]=[CH:15][N+:12]([O-:14])=[O:13]

参加物

5

反応物 3

HCID 6375NitromethaneHCID 517165Ammonium AcetateHCID 27348722-Fluoro-5-methoxybenzaldehyde

生成物 1

HCID 66692011HCID 66692011、化合物収率 97.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Heat 2-fluoro-5-methoxybenzaldehyde (15 g, 97.4 mmol) with nitromethane (32 mL, 584 mmol) and ammonium acetate (30 g, 390 mmol) in acetic acid (136 mL) under reflux for 30 min. Evaporate the solvent and dissolve the residue in ether. Wash the organic fraction with water, saturated aqueous NaHCO3 and evaporate to give the desired intermediate (18.7 g, 97%). GC-MS m/z: 197 (M)+.

後処理

  1. temperatureunder reflux for 30 min
  2. customEvaporate the solvent
  3. dissolutiondissolve the residue in ether
  4. washWash the organic fraction with water, saturated aqueous NaHCO3
  5. customevaporate

出典と根拠

ORDレコード
ord-ffb1f75d75994092939b37275cd9e508
出典データセット
uspto-grants-2013_11
特許番号
US08580780B2

反応ノート

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