Sodium Sulfite → 4-[2,2,2-trifluoro-1-(triethylsilyloxy)ethyl]pyridine N-oxide

HRID 1880761ノート

反応式

HRID 1880761 の反応式
[F:1][C:2]([F:19])([F:18])[CH:3]([C:12]1[CH:17]=[CH:16][N:15]=[CH:14][CH:13]=1)[O:4][Si:5]([CH2:10][CH3:11])([CH2:8][CH3:9])[CH2:6][CH3:7].ClC1C=CC=C(C(OO)=[O:28])C=1.S([O-])([O-])=O.[Na+].[Na+]>C(Cl)(Cl)Cl>[F:19][C:2]([F:18])([F:1])[CH:3]([C:12]1[CH:17]=[CH:16][N+:15]([O-:28])=[CH:14][CH:13]=1)[O:4][Si:5]([CH2:8][CH3:9])([CH2:6][CH3:7])[CH2:10][CH3:11]

参加物

5

反応物 3

HCID 24437Sodium SulfiteHCID 70297m-Chloroperbenzoic acidHCID 595702944-[2,2,2-Trifluoro-1-(triethylsilyloxy)ethyl]pyridine

生成物 1

HCID 595703784-[2,2,2-trifluoro-1-(triethylsilyloxy)ethyl]pyridine N-oxide収率 86.2%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
0 °C

実験手順

To 40 ml of chloroform were added 5.5 g of 4-[2,2,2-trifluoro-1-(triethylsilyloxy)ethyl]pyridine, and 7.5 g of meta-chloroperbenzoic acid, and the mixture was stirred at 0° C. for 2 hours, and at room temperature for 3 hours. Thereafter, the reaction solution was poured into an aqueous saturated sodium sulfite solution, followed by extraction with chloroform three times. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 5 g of 4-[2,2,2-trifluoro-1-(triethylsilyloxy)ethyl]pyridine N-oxide.

後処理

  1. waitat room temperature for 3 hours
  2. extractionfollowed by extraction with chloroform three times
  3. washwashed with an aqueous saturated sodium chloride solution
  4. dry with materialdried with anhydrous magnesium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-8472f885485a498c8d70d7349187b95d
出典データセット
uspto-grants-2012_11
特許番号
US08318776B2

反応ノート

読み込み中…