Aluminum(III) Chloride → HCID 68676527, 화합물

HRID 2233018노트

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HRID 2233018 반응식
C([N:5]1[C:18](=[O:19])[N:8]2[CH:9]=[C:10]([C:14]([CH3:17])([CH3:16])[CH3:15])[N:11]=[C:12]([Cl:13])[C:7]2=[N:6]1)(C)(C)C.[Cl-].[Cl-].[Cl-].[Al+3]>ClCCCl>[C:14]([C:10]1[N:11]=[C:12]([Cl:13])[C:7]2[N:8]([C:18](=[O:19])[NH:5][N:6]=2)[CH:9]=1)([CH3:17])([CH3:15])[CH3:16]

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 68678410HCID 68678410, 화합물

생성물 1

HCID 68676527HCID 68676527, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

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온도
80 °C

실험 절차

A solution of 4.10 g of the product of Step E in 1,2-dichloroethane (142 mL) was treated with 5.60 g of aluminum trichloride and the suspension was heated to 80° C. After two h, the reaction mixture was cooled to ambient temperature and poured into ice water (500 g). After the ice had dissolved, the mixture was extracted with EtOAc and the organic layer was washed with sat. sodium chloride solution, dried over magnesium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography to afford 6-tert-butyl-8-chloro-2H-[1,2,4]triazolo[4,3-a]pyrazin-3-one as a yellow solid. MS (M+H+)=227.3.

후처리

  1. temperatureAfter two h, the reaction mixture was cooled to ambient temperature
  2. extractionthe mixture was extracted with EtOAc
  3. washthe organic layer was washed with sat. sodium chloride solution
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe residue was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-aca4f55900ba465889a136bd4e5c9cf8
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07709473B2

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