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

HRID 1880761노트

반응식

HRID 1880761 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8472f885485a498c8d70d7349187b95d
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318776B2

반응 노트

불러오는 중…