Water → 2-Chloro-4-methyl-6-phenyl-1,3,5-triazine

HRID 635893

反応式

HRID 635893 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=1.[CH3:15][Mg]Br.O1CCCC1.O>O1CCCC1>[Cl:1][C:2]1[N:7]=[C:6]([CH3:15])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[N:3]=1

参加物

5

反応物 3

HCID 962WaterHCID 155492,4-Dichloro-6-phenyl-1,3,5-triazineHCID 178420675HCID 178420675、化合物

生成物 1

HCID 356892-Chloro-4-methyl-6-phenyl-1,3,5-triazine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

(Step 2) In 85 ml of dry tetrahydrofuran was dissolved 17 g of 2,4-dichloro-6-phenyl-1,3,5-triazine. To this solution on an ice-water bath was added 135 ml of 1M methylmagnesium bromide-tetrahydrofuran dropwise over about 30 minutes. After completion of dropwise addition, the mixture was stirred at room temperature for 2 hours. This reaction mixture was poured into iced water and extracted with ethyl acetate. The extract was washed with water, dried over MgSO4, and concentrated. The residue was purified with silica gel column chromatography to provide 3.6 g of the title compound as white crystals.

後処理

  1. additionAfter completion of dropwise addition
  2. extractionextracted with ethyl acetate
  3. washThe extract was washed with water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe residue was purified with silica gel column chromatography

出典と根拠

ORDレコード
ord-d0135db25a814c05a50342020495c5f3
出典データセット
uspto-grants-2001_02
特許番号
US06191149B1

関連ノート

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