Chloroform → HCID 21199122、化合物

HRID 1066282

反応式

HRID 1066282 の反応式
[CH3:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:3]=1[C:4]#[N:5].[Br:11]Br.C(Cl)(Cl)Cl.[Al+3].[Cl-].[Cl-].[Cl-]>O>[Br:11][C:9]1[C:2]([CH3:1])=[C:3]([C:6]([CH3:10])=[CH:7][CH:8]=1)[C:4]#[N:5]

参加物

6

反応物 4

HCID 6212ChloroformHCID 24408BromineHCID 810572,6-DimethylbenzonitrileHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 21199122HCID 21199122、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 2,6-dimethylbenzonitrile (5.0 g, 38.0 mmol), bromine (1.9 ml, 38.0 mmol) and chloroform (10 ml) is stirred at room temperature for 24 hours and subsequently heated to 60° C. for 6 hours. Upon cooling down to 0° C., 10 g of AlCl3 are added and the mixture is stirred for 4 hours at 0° C. The reaction mixture is poured into water and extracted with toluene. The organic phase is separated and concentrated and the residue is purified by column chromatography yielding the pure product as brown crystals, 6.2 g, mp. 60° C.

後処理

  1. temperaturesubsequently heated to 60° C. for 6 hours
  2. temperatureUpon cooling down to 0° C.
  3. stirringthe mixture is stirred for 4 hours at 0° C
  4. extractionextracted with toluene
  5. customThe organic phase is separated
  6. concentrationconcentrated
  7. customthe residue is purified by column chromatography

出典と根拠

ORDレコード
ord-c743b4deb59541ecad943013fd7950f7
出典データセット
uspto-grants-2001_06
特許番号
US06242498B1

関連ノート

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