Boron trifluoride etherate → 2-tert-Butyl-4-(pyrid-3-yl)-5-(2-bromophenyl)-1,3-dioxolane

HRID 1613648ノート

反応式

HRID 1613648 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]([OH:17])(O)[CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Br:15])[CH:2]=1.[CH3:18][C:19]([CH:22]=[O:23])([CH3:21])[CH3:20].B(F)(F)F.CCOCC.C([O-])(O)=O.[Na+]>C(Cl)Cl>[C:19]([CH:22]1[O:17][CH:7]([C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)[CH:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[Br:15])[O:23]1)([CH3:21])([CH3:20])[CH3:18]

参加物

6

反応物 4

HCID 8000Boron trifluoride etherateHCID 12417PivalaldehydeHCID 516892Sodium BicarbonateHCID 197741971-(Pyrid-3-yl)-2-(2-bromophenyl)-ethanediol

生成物 1

HCID 197741992-tert-Butyl-4-(pyrid-3-yl)-5-(2-bromophenyl)-1,3-dioxolane

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

8 g (0.027 mol) of 1-(pyrid-3-yl)-2-(2-bromophenyl)-ethanediol and 4.5 g (0.0525 mol) of pivaldehyde were dissolved in 100 ml of methylene chloride. This was achieved by adding 4.35 ml (0.0525 mol) of boron trifluoride etherate dropwise at room temperature and stirring overnight. Thereafter, the mixture was poured onto ice water and was neutralized with NaHCO3 solution. The organic phase was washed with water, dried over Na2SO4 and filtered, and the filtrate was evaporated down. The crude product was purified by chromatography.

後処理

  1. additionThereafter, the mixture was poured onto ice water
  2. washThe organic phase was washed with water
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customthe filtrate was evaporated down
  6. customThe crude product was purified by chromatography

出典と根拠

ORDレコード
ord-fd7d379506b446dc8fd996a227ed1ff7
出典データセット
uspto-grants-1993_03
特許番号
US05194441

反応ノート

読み込み中…