Hydrochloric Acid → HCID 22013535、化合物

HRID 485557ノート

反応式

HRID 485557 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 22013535HCID 22013535、化合物

試薬・触媒・溶媒 2

HCID 24014Cupric Chloride触媒HCID 6342Acetonitrile溶媒2 回

実験手順

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 2N aqueous hydrochloric acid and extracted with two 150 ml portions of diethyl ether. The extracts were combined, washed with 200 ml of 2N 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).

後処理

  1. waitroom temperature for two days
  2. extractionextracted with two 150 ml portions of diethyl ether
  3. washwashed with 200 ml of 2N 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

出典と根拠

ORDレコード
ord-a091e6190d7b4136b997ea7b9c65e7f0
出典データセット
uspto-grants-1985_08
特許番号
US04536591

反応ノート

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