Chloroform → HCID 21199122, 화합물

HRID 1066282

반응식

HRID 1066282 반응식
[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]

참가 물질

6

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c743b4deb59541ecad943013fd7950f7
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06242498B1

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