Nitromethane → HCID 66692011, 화합물

HRID 2041108노트

반응식

HRID 2041108 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 66692011HCID 66692011, 화합물수율 97.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-ffb1f75d75994092939b37275cd9e508
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08580780B2

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