Sulfur → 4-tert-Butyl-1-benzofuran-5-ol
反応式
C([C:5]1[O:6][C:7]2[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][C:8]=2[CH:9]=1)(C)(C)C.[S]>>[C:8]([C:10]1[C:8]2[CH:9]=[CH:5][O:6][C:7]=2[CH:13]=[CH:12][C:11]=1[OH:14])([CH3:10])([CH3:9])[CH3:7]参加物
3
反応条件
- 温度
- 225 °C
実験手順
A mixture of 4 tert butyl-4,5,6,7 tetrahydro-5-benzofuranone (1.00 g, 5.2 mmol) and sulfur (0.167 g, 1 equivalent) in a sealable tube is flushed with nitrogen, sealed and heated to 225° C. for 30 minutes. An additional portion of sulfur (0.030 g) is then added and the mixture heated an additional 15 minutes. After cooling the total reaction mixture is taken up in a small portion of methylene chloride and applied directly to a flash silica gel column. Elution with 5% ethyl acetate in hexane gives 4-tert-butyl5-benzofuranol.
後処理
- customis flushed with nitrogen
- customsealed
- additionAn additional portion of sulfur (0.030 g) is then added
- temperaturethe mixture heated an additional 15 minutes
- temperatureAfter cooling the total reaction mixture
- washElution with 5% ethyl acetate in hexane
出典と根拠
- ORDレコード
- ord-460ae84ccb5642d0a2d60187e0daf816
- 出典データセット
- uspto-grants-1990_10
- 特許番号
- US04966907
反応ノート
読み込み中…