Sodium Carbonate → 3-Iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine 1-oxide

HRID 628012

반응식

HRID 628012 반응식
ClC1C=CC=C(C(OO)=[O:9])C=1.[I:12][C:13]1[CH:14]=[N:15][CH:16]=[CH:17][C:18]=1[O:19][CH2:20][CH2:21][C:22]1[CH:26]=[CH:25][S:24][CH:23]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(Cl)Cl>[I:12][C:13]1[CH:14]=[N+:15]([O-:9])[CH:16]=[CH:17][C:18]=1[O:19][CH2:20][CH2:21][C:22]1[CH:26]=[CH:25][S:24][CH:23]=1

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 70297m-Chloroperbenzoic acidHCID 579002113-Iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine

생성물 1

HCID 582840413-Iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine 1-oxide수율 96.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

m-Chloroperbenzoic acid (1.55 g, 6.29 mmol) was added portionwise to a solution of 1.0 g (3.02 mmol) of 3-iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine in 150 ml of methylene chloride. The mixture was stirred for 18 hours then mixed with 100 ml of 1 M aqueous sodium carbonate. The organic layer was separated and the aqueous one was extracted 2 times with 10 ml of methylene chloride. Combined organic extracts were washed with brine and dried over sodium sulfate. The solution was concentrated in vacuum to give 3-iodo-4-(2-(thiophen-3-yl)ethoxy)pyridine 1-oxide (1.01 g, 92%). MS: (ESI+) 348.0

후처리

  1. customThe organic layer was separated
  2. extractionthe aqueous one was extracted 2 times with 10 ml of methylene chloride
  3. washCombined organic extracts were washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationThe solution was concentrated in vacuum

출처 및 근거

ORD 기록
ord-bb7485e41aca4e91974363d6d971d27c
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09309265B2

연결된 노트

불러오는 중…