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

HRID 745142

반응식

HRID 745142 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-abbfb463c6e041c4aa74df0d48b07a2c
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04597891

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