Acetic Acid → Acetamide, N-(2-methoxy-5-nitrophenyl)-

HRID 273936

반응식

HRID 273936 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[O:11][CH3:12].[C:13](O)(=[O:15])[CH3:14].C(OC(=O)C)(=O)C>O>[C:13]([NH:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[O:11][CH3:12])(=[O:15])[CH3:14]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 74472-Methoxy-5-nitroanilineHCID 7918Acetic Anhydride

생성물 1

HCID 97239Acetamide, N-(2-methoxy-5-nitrophenyl)-

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

504 g (3 mol) of 2-amino-4-nitro-1-methoxybenzene are introduced into 860 ml of acetic acid and 600 ml of water (or the combined main filtrate and first wash filtrate of a previous batch) and the mixture is heated to 80° C. 358 g (3.2 mol) of acetic anhydride are added dropwise in the course of 10 minutes. The mixture is subsequently stirred at 80° C. for 4 hours, and then cooled to room temperature, while stirring, by removing the heating bath and finally to 15° C. The pale yellow needles which have precipitated are filtered off with suction, washed with 300 ml of 60% strength acetic acid and 1500 ml of water in several portions and dried.

후처리

  1. temperaturecooled to room temperature
  2. stirringwhile stirring
  3. customby removing the heating bath
  4. customfinally to 15° C
  5. customThe pale yellow needles which have precipitated
  6. filtrationare filtered off with suction
  7. washwashed with 300 ml of 60% strength acetic acid and 1500 ml of water in several portions
  8. customdried

출처 및 근거

ORD 기록
ord-81e010c1cada4efabc4550a7a913a1fe
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05387716

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