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

HRID 1647170ノート

反応式

HRID 1647170 の反応式
[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]

参加物

5

反応物 3

HCID 70297m-Chloroperbenzoic acid2 回HCID 516892Sodium BicarbonateHCID 199264514-Methyl-[1,3]dioxolo[4,5-c]pyridine

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-919326a2a7f34a9ba3ad64fc9709fe5c
出典データセット
uspto-grants-1995_07
特許番号
US05430042

反応ノート

読み込み中…