Sulfuric Acid → HCID 19825785、化合物

HRID 2249210ノート

反応式

HRID 2249210 の反応式
S(=O)(=O)(O)O.O[C:7]([CH:10]1[CH2:14][C:13]2[CH:15]=[C:16]([OH:21])[C:17]([O:19][CH3:20])=[CH:18][C:12]=2[O:11]1)([CH3:9])[CH3:8]>>[OH:21][C:16]1[C:17]([O:19][CH3:20])=[CH:18][C:12]2[O:11][C:10]([CH:7]([CH3:9])[CH3:8])=[CH:14][C:13]=2[CH:15]=1

参加物

3

反応物 2

HCID 1118Sulfuric AcidHCID 19825784HCID 19825784、化合物

生成物 1

HCID 19825785HCID 19825785、化合物収率 43.5%

実験手順

To a solution of conc. sulfuric acid (1 ml) was added 2,3-dihydro-2-(1-hydroxy-1-methylethyl)-6-methoxy-5-benzofuranol (50 mg) in several portions during a period of few minutes. The mixture was stirred for 10 minutes at ambient temperature and poured into ice water. The separated oil was extracted with methylene chloride. The organic layer was washed with water, dried, and concentrated in vacuo. The residue was purified by column chromatography on silica gel (n-hexane/methylene chloride =1/1) to yield 5-hydroxy-6-methoxy-2-(1-methylethyl)benzofuran (20 mg) as crystals.

後処理

  1. extractionThe separated oil was extracted with methylene chloride
  2. washThe organic layer was washed with water
  3. customdried
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by column chromatography on silica gel (n-hexane/methylene chloride =1/1)

出典と根拠

ORDレコード
ord-41ac6b771af64590ad03b6e1d14da17b
出典データセット
uspto-grants-1991_08
特許番号
US05043354

反応ノート

読み込み中…