Hydrochloric Acid → (1,1'-Biphenyl)-4,4'-diamine, 2,2'-bis(trifluoromethyl)-

HRID 745142

反応式

HRID 745142 の反応式
[F:1][C:2]([F:26])([F:25])[C:3]1[CH:8]=[C:7]([N+:9]([O-])=O)[CH:6]=[CH:5][C:4]=1[C:12]1[CH:17]=[CH:16][C:15]([N+:18]([O-])=O)=[CH:14][C:13]=1[C:21]([F:24])([F:23])[F:22].Cl>C(O)C>[F:1][C:2]([F:25])([F:26])[C:3]1[CH:8]=[C:7]([NH2:9])[CH:6]=[CH:5][C:4]=1[C:12]1[CH:17]=[CH:16][C:15]([NH2:18])=[CH:14][C:13]=1[C:21]([F:22])([F:23])[F:24]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 113724052,2'-Bis(trifluoromethyl)-4,4'-dinitrobiphenyl

生成物 1

HCID 629349(1,1'-Biphenyl)-4,4'-diamine, 2,2'-bis(trifluoromethyl)-

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Stannous chloride dihydrate (8 g) was added to a solution of 2,2'-bis(trifluoromethyl)-4,4'-dinitro-1,1'-biphenyl (1.9 g) in 5 ml of ethanol. Concentrated hydrochloric acid (12 ml) was added carefully to the mixture while stirring at room temperature. The mixture was refluxed overnight and the ethanol was removed. Water was added to the residue and it was made basic with 20% sodium hydroxide solution. The resulting white precipitate was collected by filtration, washed with water, dried and then extracted in a Soxhlet flask with acetone for four hours. Removal of acetone gave a white residue, 2,2'-bis(trifluoromethyl)-4,4'-diamino-1,1'-biphenyl, ##STR7## which was recrystallized from chloroform-hexane to give 1.2 g (74% yield) of short white needles, m.p. 185°-186° C.

後処理

  1. temperatureThe mixture was refluxed overnight
  2. customthe ethanol was removed
  3. additionWater was added to the residue and it
  4. filtrationThe resulting white precipitate was collected by filtration
  5. washwashed with water
  6. customdried
  7. extractionextracted in a Soxhlet flask with acetone for four hours
  8. customRemoval of acetone

出典と根拠

ORDレコード
ord-abbfb463c6e041c4aa74df0d48b07a2c
出典データセット
uspto-grants-1986_07
特許番号
US04597891

関連ノート

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