m-Chloroperbenzoic acid → 4-Methyl-5-oxido-[1,3]dioxolo[4,5-c]pyridin-5-ium

HRID 1647170노트

반응식

HRID 1647170 반응식
[CH3:1][C:2]1[C:7]2[O:8][CH2:9][O:10][C:6]=2[CH:5]=[CH:4][N:3]=1.C(=O)([O-])[OH:12].[Na+].C1C=C(Cl)C=C(C(OO)=O)C=1>C(Cl)Cl>[CH3:1][C:2]1[C:7]2[O:8][CH2:9][O:10][C:6]=2[CH:5]=[CH:4][N+:3]=1[O-:12]

참가 물질

5

반응물 3

HCID 70297m-Chloroperbenzoic acid2회HCID 516892Sodium BicarbonateHCID 199264514-Methyl-[1,3]dioxolo[4,5-c]pyridine

생성물 1

HCID 199264794-Methyl-5-oxido-[1,3]dioxolo[4,5-c]pyridin-5-ium

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To the methylene chloride solution of 2-methyl-3,4-methylenedioxypyridine from example I 21 sodium hydrogen carbonate (1M, 50 ml) and MCPBA (4 g, 70%) were added. The mixture was stirred at ambient temperature for 15 min whereupon the excess of MCPBA was destroyed with addition of sodium thiosulphate (1 g). The organic phase was separated and the aqueous phase was extracted with methylene chloride (3×50 ml). The collected organic phases were concentrated under reduced pressure and chromatographed on silica (CH2Cl2 /MeOH, 90:10). Yield: 120 mg (7,8%) of the title compound.

후처리

  1. customwas destroyed with addition of sodium thiosulphate (1 g)
  2. customThe organic phase was separated
  3. extractionthe aqueous phase was extracted with methylene chloride (3×50 ml)
  4. concentrationThe collected organic phases were concentrated under reduced pressure
  5. customchromatographed on silica (CH2Cl2 /MeOH, 90:10)

출처 및 근거

ORD 기록
ord-919326a2a7f34a9ba3ad64fc9709fe5c
출처 데이터셋
uspto-grants-1995_07
특허 번호
US05430042

반응 노트

불러오는 중…