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

HRID 273936

反応式

HRID 273936 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-81e010c1cada4efabc4550a7a913a1fe
出典データセット
uspto-grants-1995_02
特許番号
US05387716

関連ノート

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