Sodium borohydride → HCID 21476897、化合物

HRID 2293582ノート

反応式

HRID 2293582 の反応式
[CH:1]([C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][C:4]=1[CH2:13][CH2:14][CH3:15])=[O:2].[BH4-].[Na+]>CO>[OH:2][CH2:1][C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9][CH3:10])=[O:8])=[CH:5][C:4]=1[CH2:13][CH2:14][CH3:15]

参加物

4

反応物 2

HCID 4311764Sodium borohydride2 回HCID 21476898HCID 21476898、化合物

生成物 1

HCID 21476897HCID 21476897、化合物収率 66.2%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of 0.609 g (2.96 mmol) of the product of Step C dissolved in 10 mL of methanol was added 0.056 g (1.48 mmol) of sodium borohydride in small portions as the reaction mixture was stirred at room temperature under a nitrogen atmosphere. After stirring for 30 minutes the excess sodium borohydride was quenched by addition of 10% aqueous NaHSO4. The methanol was removed in vacuo, and the residue was partitioned between EtOAc and water. The organic layer was separated, dried (MgSO4), filtered and evaporated. The residue was then purified on a silica gel flash chromatography column eluted with 20% EtOAc-hexane; evaporation of the purified fractions and drying in vacuo afforded 0.408 g (66%) of the title compound.

後処理

  1. customwas quenched by addition of 10% aqueous NaHSO4
  2. customThe methanol was removed in vacuo
  3. customthe residue was partitioned between EtOAc and water
  4. customThe organic layer was separated
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated
  8. customThe residue was then purified on a silica gel flash chromatography column
  9. washeluted with 20% EtOAc-hexane
  10. customevaporation of the purified fractions
  11. customdrying in vacuo

出典と根拠

ORDレコード
ord-99d17b48bd9b4aeba03a9d1d2795067d
出典データセット
uspto-grants-1997_11
特許番号
US05686478

反応ノート

読み込み中…