反応 #2254171

ord-2495ae740b9140b7a78e5059f475cd15

反応方程式

[BH4-].[Na+]
sodium borohydride
CCO
ethanol
CCOC(=O)c1cc(=O)c2ccc(O)cc2o1
Ethyl 7-hydroxychromen-4-one-2-carboxylate
[Ca+2].[Cl-].[Cl-]
calcium chloride
[BH4-].[Na+]
Sodium borohydride
COc1cc(=O)c2ccc(O)cc2o1
2-methoxy-7-hydroxy-4H-chromen-4-one

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度again cooled
  2. 2
    workup.STIRRINGThe mixture is stirred overnight at RT

実験手順

Ethyl 7-hydroxychromen-4-one-2-carboxylate (2 g, 8.538 mmol) and granulated and dried calcium chloride (1 g, 9.01 mmol) are initially introduced, and ethanol (absolute, 40 ml) is added. Sodium borohydride (1.33 g, 35.157 mmol) is subsequently added in portions with ice cooling. The reaction mixture is stirred at RT for 2 hours, then again cooled using an ice bath, and sodium borohydride (0.45 g, 11.895 mmol) is again added. The mixture is stirred overnight at RT.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09044409B2uspto-grants-2015_06