Sodium Hydroxide → HCID 23469722、化合物

HRID 128464

反応式

HRID 128464 の反応式
Cl.[F:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][NH2:10].[OH-].[Na+].CN([CH:16]=[N:17][C:18](=O)[C:19]1[CH:24]=[CH:23][C:22]([N+:25]([O-:27])=[O:26])=[CH:21][CH:20]=1)C>O.O1CCOCC1.C(O)(=O)C>[F:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[C:18]([C:19]2[CH:20]=[CH:21][C:22]([N+:25]([O-:27])=[O:26])=[CH:23][CH:24]=2)=[N:17][CH:16]=[N:10]1

参加物

7

反応物 3

HCID 14798Sodium HydroxideHCID 2723910Hydrazine, (2-fluorophenyl)-, hydrochloride (1:1)HCID 12550338HCID 12550338、化合物

生成物 1

HCID 23469722HCID 23469722、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒2 回

実験手順

A 25.0 g. portion of o-fluorophenylhydrazine hydrochloride is dissolved in 150 ml. of p-dioxane with warming and 31.0 ml. of 5 N sodium hydroxide is added. After solution is complete, 80 ml. of glacial acetic acid and 210 ml. of water are added followed by 28.1 g. of N-(dimethylaminomethylene)-p-nitrobenzamide in 100 ml. of warm p-dioxane. This reaction mixture is heated at 90°-95° C. for 1.5 hours, then cooled and poured into 1500 ml. of water. The solid is collected by filtration, washed with water, dried and crystallized from 200 ml. of ethanol, giving 13.9 g. of the desired product as a tan solid, mp. 143°-145° C.

後処理

  1. temperatureThis reaction mixture is heated at 90°-95° C. for 1.5 hours
  2. temperaturecooled
  3. additionpoured into 1500 ml
  4. filtrationThe solid is collected by filtration
  5. washwashed with water
  6. customdried
  7. customcrystallized from 200 ml
  8. customof ethanol, giving 13.9 g

出典と根拠

ORDレコード
ord-769e086f96e04461b8f8105605192835
出典データセット
uspto-grants-1981_03
特許番号
US04259504

関連ノート

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