Aniline → 2-(2-Methylthioethoxy)-phenylhydrazine

HRID 4243

反応式

HRID 4243 の反応式
[NH2:1]C1C=CC=CC=1.[CH3:8][S:9][CH2:10][CH2:11][O:12][C:13]1[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=1[NH2:15].N([O-])=O.[Na+].O.O.Cl[Sn]Cl.[OH-].[Na+]>O.Cl.CCOCC.C(O)(=O)C>[CH3:8][S:9][CH2:10][CH2:11][O:12][C:13]1[CH:19]=[CH:18][CH:17]=[CH:16][C:14]=1[NH:15][NH2:1]

参加物

10

反応物 5

HCID 6115AnilineHCID 14798Sodium HydroxideHCID 61436Stannous chloride dihydrateHCID 23668193Sodium NitriteHCID 542131632-(2-Methylthioethoxy)aniline

生成物 1

HCID 542892902-(2-Methylthioethoxy)-phenylhydrazine

試薬・触媒・溶媒 4

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒2 回HCID 962Water溶媒3 回HCID 3283Diethyl Ether溶媒

実験手順

27.4 g of the aniline obtained under (b) are placed into 45 ml of glacial acetic acid and, with ice cooling, a mixture of 37 ml of concentrated HCl and 75 ml of H2O is added. The formed suspension is diazotised at 0°-5° C. with 10.3 g of NaNO2 in 22 ml of water. The diazonium solution is subsequently stirred at 0° C. for 10 minutes, and a solution of 80.7 g of SnCl2.2H2O in 112 ml of concentrated HCl is then quickly added with cooling. After 4 hours, water is added to the reaction mixture, and extraction is repeatedly performed with ether. The aqueous phase is afterwards rendered alkaline with a 10% aqueous sodium hydroxide solution, and extracted three times with ether. After customary further processing of the ether phases, there is obtained the compound of the formula ##STR61## having a melting point of 72.5°-74.5° C.

後処理

  1. additionis added
  2. temperaturewith cooling
  3. extractionextracted three times with ether
  4. customAfter customary further processing of the ether phases, there is obtained the compound of the formula

出典と根拠

ORDレコード
ord-8ff8d568cf1248518f7da91bcabe7759
出典データセット
uspto-grants-1988_02
特許番号
US04725302

関連ノート

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