Acetic Anhydride → 1,3-Dioxolo[4,5-C]pyridine-4-methanol

HRID 1647171ノート

反応式

HRID 1647171 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[O-].C(OC(=O)C)(=[O:14])C>>[OH:14][CH2:1][C:2]1[C:7]2[O:8][CH2:9][O:10][C:6]=2[CH:5]=[CH:4][N:3]=1

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 199264794-Methyl-5-oxido-[1,3]dioxolo[4,5-c]pyridin-5-ium

生成物 1

HCID 199264631,3-Dioxolo[4,5-C]pyridine-4-methanol

反応条件

温度
110 °C

実験手順

2-Methyl-3,4-methylenedioxypyridine-N-oxide (120 mg, 0.78 mmol) was dissolved in acetic anhydride (10 ml) and the solution was heated at 110° C. for 15 min, whereupon the mixture was concentrated under reduced pressure. The residue was dissolved in methanol (20 ml) and sodium hydroxide (3 drops, 6M) was added. After 30 min at ambient temperature the mixture was neutralised with acetic acid (pH 6) and concentrated under reduced pressure. The residue was chromatographed on silica (hexane/ethyl acetate, 1:1). Yield: 90 mg (75%) of the title compound.

後処理

  1. concentrationwas concentrated under reduced pressure
  2. dissolutionThe residue was dissolved in methanol (20 ml)
  3. additionsodium hydroxide (3 drops, 6M) was added
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was chromatographed on silica (hexane/ethyl acetate, 1:1)

出典と根拠

ORDレコード
ord-28f7757c3aa948fe8410877b4c17c695
出典データセット
uspto-grants-1995_07
特許番号
US05430042

反応ノート

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