Sulfuric Acid → N-Nitrosodiphenylamine

HRID 867145

反応式

HRID 867145 の反応式
[C:1]1([NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N:14]([O-])=[O:15].[Na+].S(=O)(=O)(O)O>ClC=C(Cl)Cl>[N:14]([N:7]([C:1]1[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1)[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)=[O:15]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 11487Diphenylamine2 回HCID 23668193Sodium Nitrite

生成物 1

HCID 6838N-Nitrosodiphenylamine

試薬・触媒・溶媒 1

HCID 6575Trichloroethylene溶媒

実験手順

210 g of 20% diphenylamine solution in trichloroethylene, 59 g of 38% sodium nitrite aqueous solution and 150 g of 20% sulfuric acid are simultaneously fed, under stirring, (Re = 8-10×103) at 17°-20° C. for about 7-10 min into a 500 ml reactor equipped with a cooling jacket, a thermometer and an agitator; this is followed by another stirring for about 5-8 min. The stirring is discontinued after said period of time has elapsed; complete layer separation of the organic and aqueous phases takes place during 15-20 min. 217 g of organic phase containing 48.4 g of N-nitrosodiphenylamine and 0.42 g of diphenylamine are obtained. Diphenylamine conversion degree is 99%; N-nitrosodiphenylamine yield, 99.3% in terms of converted diphenylamine.

後処理

  1. custom(Re = 8-10×103) at 17°-20° C. for about 7-10 min into a 500 ml reactor equipped with a cooling jacket
  2. customstirring for about 5-8 min
  3. waitafter said period of time
  4. customcomplete layer separation of the organic and aqueous phases
  5. customduring 15-20 min
  6. addition217 g of organic phase containing 48.4 g of N-nitrosodiphenylamine and 0.42 g of diphenylamine
  7. customare obtained

出典と根拠

ORDレコード
ord-0108dc8559bf40fa88541d969f5a54cf
出典データセット
uspto-grants-1978_07
特許番号
US04102926

関連ノート

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