Hydrochloric Acid → HCID 22013535, 화합물

HRID 1065576노트

반응식

HRID 1065576 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:3]=1N.N(OCCC(C)C)=O.[ClH:23]>C(#N)C.[Cu](Cl)Cl>[Cl:23][C:3]1[C:2]([CH3:1])=[CH:7][CH:6]=[CH:5][C:4]=1[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 8053Isoamyl NitriteHCID 6030842-amino-3-methylbiphenyl

생성물 1

HCID 22013535HCID 22013535, 화합물

시약·촉매·용매 2

HCID 24014Cupric Chloride촉매HCID 6342Acetonitrile용매2회

실험 절차

During a five minute period a solution of 3-methyl-[1,1'-biphenyl]-2-amine (5.8 g, 0.0316 mole) in 15 ml of dry acetonitrile was added to a stirred mixture of anhydrous copper (II) chloride (7.5 g, 0.038 mole) and isoamyl nitrite (5.55 g, 0.0474 mole) in 100 ml of anhydrous acetonitrile. The reaction mixture was stirred at room temperature for two hours, 65° for two hours, then room temperature for two days. The mixture was diluted with 600 ml of 2 N aqueous hydrochloric acid and extracted with two 150 ml portions of diethyl ether. The extracts were combined, washed with 200 ml of 2 N aqueous hydrochloric acid, and dried over anhydrous magnesium sulfate. The mixture was filtered and the filtrate evaporated under reduced pressure to give an oil. The oil was purified by column chromatography on silica gel to give 2-chloro-3-methyl-[1,1'-biphenyl] (0.4 g).

후처리

  1. waitroom temperature for two days
  2. extractionextracted with two 150 ml portions of diethyl ether
  3. washwashed with 200 ml of 2 N aqueous hydrochloric acid
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationThe mixture was filtered
  6. customthe filtrate evaporated under reduced pressure
  7. customto give an oil
  8. customThe oil was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-2b880b9ff45e4f10aa5619c9e43236b1
출처 데이터셋
uspto-grants-1982_05
특허 번호
US04329518

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