反応 #2336522

ord-b042792eae154febbebc73d32bd28eb2

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄washed with 5% HCl (20 mL)
  2. 2
    乾燥The organic layer was dried over MgSO4
  3. 3
    ろ過filtered
  4. 4
    濃縮concentrated
  5. 5
    その他The residue was purified via flash chromatography

実験手順

Toluenesulfonyl chloride (397 mg, 2.08 mmol) was added to a 0° C. solution of 7-furyl-3-methyl-4-chromanone oxime (61) (461 mg, 1.89 mmol) and pyridine (0.5 mL) in CH2Cl2 (10 mL). After 6 hours, the mixture was diluted with CH2Cl2 (30 mL) and washed with 5% HCl (20 mL). The organic layer was dried over MgSO4, filtered and concentrated. The residue was purified via flash chromatography using 5:1 hexanes:EtOAc as the eluent, to provide 7-furyl-3-methyl-4-chromanone O-(toluenesulfonyl)-oxime (62) (429 mg) as a pink solid, m.p. 163-164° C. (dec).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE039991E1uspto-grants-2008_01