Azoxybenzene → 1,2-Bis(3-chlorophenyl)hydrazine

HRID 616560

反応式

HRID 616560 の反応式
[SH-].[Na+].Cl[C:4]1[CH:9]=[CH:8][C:7]([Cl:10])=[CH:6][C:5]=1[N+:11](=[N:13][C:14]1[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][C:15]=1Cl)[O-].[N+](C1C=CC=CC=1)(=NC1C=CC=CC=1)[O-]>CO>[Cl:10][C:7]1[CH:8]=[CH:9][CH:4]=[C:5]([NH:11][NH:13][C:14]2[CH:19]=[C:18]([Cl:20])[CH:17]=[CH:16][CH:15]=2)[CH:6]=1

参加物

5

反応物 3

HCID 10316AzoxybenzeneHCID 28015Sodium hydrosulfideHCID 14205666Diazene, bis(2,5-dichlorophenyl)-, 1-oxide

生成物 1

HCID 2579191,2-Bis(3-chlorophenyl)hydrazine収率 76%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
70 °C

実験手順

85 Parts of an aqueous solution of technical sodium hydrosulfide containing 35 percent NaHS and 9 percent Na2S 2 O3 were added to a mixture comprising 65.4 parts of 2,2'-dichlor-5,5'-dichloroazoxybenzene in 196 parts of methanol at room temperature within 90 minutes. The reaction mixture was then refluxed at 70° C to75° C for a period of 5 hours. The pH had been kept between 9 and 9.4. After this period the starting azoxybenzene was shown to be all consumed and the reaction mixture was cooled down to 0° C to 5° C, and the resulting precipitate filtered off and washed with water until alkali-free. After drying below 70° C 48 parts of 2,2'-dichloro,-5,5'-dichlorohydrazobenzene of a melting point of 116° C were obtained, this representing yield of 76 percent of the theory.

後処理

  1. customat room temperature
  2. customwithin 90 minutes
  3. customall consumed
  4. temperaturethe reaction mixture was cooled down to 0° C to 5° C
  5. filtrationthe resulting precipitate filtered off
  6. washwashed with water until alkali-free
  7. customAfter drying below 70° C 48 parts of 2,2'-dichloro

出典と根拠

ORDレコード
ord-16d0f3124ce94af09b5ea96fa48dc704
出典データセット
uspto-grants-1978_02
特許番号
US04075198

関連ノート

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