Methyl 4-nitrobenzoate → Benzoic acid, 4-nitro-, hydrazide

HRID 1715244

반응식

HRID 1715244 반응식
[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([C:8](OC)=[O:9])=[CH:6][CH:5]=1)([O-:3])=[O:2].O.[NH2:15][NH2:16]>CCO>[N+:1]([C:4]1[CH:13]=[CH:12][C:7]([C:8]([NH:15][NH2:16])=[O:9])=[CH:6][CH:5]=1)([O-:3])=[O:2]

참가 물질

4

반응물 2

HCID 12083Methyl 4-nitrobenzoateHCID 24654Hydrazine hydrate (1:1)

생성물 1

HCID 3693744Benzoic acid, 4-nitro-, hydrazide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Methyl 4-nitrobenzoate (5.42 g; 29.92 mmol; 1 eq.) is dissolved in EtOH (120 ml). Hydrazine hydrate (7.27 ml; 149.60 mmol; 5 eq.) is added and the mixture is stirred 1 hour at rt. It is stirred at 60° C. for 6 hours and rt overnight. The precipitate formed is filtrated and dried under vacuo, affording 4-nitrobenzohydrazide as white-off solid (4.31 g; 79%). 1H NMR (DMSO-d6) δ: 4.63 (s, 2H), 8.03 (d, J=9 Hz, 2H), 8.23 (d, J=9 Hz, 2H), 10.12 (s, 1H). HPLC (method A), Rt: 0.78 min (purity: 100.0%).

후처리

  1. stirringIt is stirred at 60° C. for 6 hours and rt overnight
  2. customThe precipitate formed
  3. filtrationis filtrated
  4. customdried under vacuo

출처 및 근거

ORD 기록
ord-c8df53604b464aae9d4f28b0d3958dc7
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07799814B2

연결된 노트

불러오는 중…