Quintozene → HCID 20065461、化合物

HRID 359600

反応式

HRID 359600 の反応式
[Cl:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([Cl:11])[C:5]([Cl:12])=[C:4]([Cl:13])[C:3]=1[Cl:14].O.[NH2:16]N>CS(C)=O>[Cl:1][C:2]1[C:7]([NH:8][NH2:16])=[C:6]([Cl:11])[C:5]([Cl:12])=[C:4]([Cl:13])[C:3]=1[Cl:14]

参加物

4

反応物 2

HCID 6720QuintozeneHCID 24654Hydrazine hydrate (1:1)

生成物 1

HCID 20065461HCID 20065461、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
25 °C

実験手順

Pentachloronitrobenzene containing 5-10% hexaxchlorobenzene, (3.0 g, 10.1 mmole) was dissolved in dimethylsulphoxide (35 ml). Hydrazine hydrate (1.25 g, 25 mmole) was added dropwise with stirring at 25° C. A slight 4°-5° C. increase in temperature was recorded and the solution became red-brown. After approximately 20 minutes a white solid began to be precipitated. Stirring was continued for one hour after which time TLC (1:1 ethyl acetate: 60°-80° C. petrol) indicated that the reaction was complete. The mixture was poured into stirred water (200 ml) and the solid filtered off and dried at 50° C. overnight. The TLC and IR was identical to an authentic sample of pentachlorophenylhydrazine. Yield=2.27 g, 80%.

後処理

  1. temperatureA slight 4°-5° C. increase in temperature
  2. customto be precipitated
  3. stirringStirring
  4. waitwas continued for one hour
  5. customafter which time TLC (1:1 ethyl acetate: 60°-80° C. petrol)
  6. additionThe mixture was poured
  7. stirringinto stirred water (200 ml)
  8. filtrationthe solid filtered off
  9. customdried at 50° C. overnight

出典と根拠

ORDレコード
ord-22cfba713da1466a820183fa4ce93ade
出典データセット
uspto-grants-1991_03
特許番号
US05001262

関連ノート

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