Aluminum(III) Chloride → HCID 68676527、化合物

HRID 2233018ノート

反応式

HRID 2233018 の反応式
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]

参加物

4

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 68678410HCID 68678410、化合物

生成物 1

HCID 68676527HCID 68676527、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aca4f55900ba465889a136bd4e5c9cf8
出典データセット
uspto-grants-2010_05
特許番号
US07709473B2

反応ノート

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