Sodium borohydride → HCID 14127272、化合物

HRID 728531ノート

反応式

HRID 728531 の反応式
[Cl:1][C:2]1([Cl:11])[C@@H:9]2[C@@H:4]([CH2:5][CH2:6][CH:7]=[CH:8]2)[C:3]1=[O:10].[BH4-].[Na+]>CO>[Cl:1][C:2]1([Cl:11])[C@@H:9]2[C@@H:4]([CH2:5][CH2:6][CH:7]=[CH:8]2)[C@H:3]1[OH:10]

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 12507348HCID 12507348、化合物2 回

生成物 1

HCID 14127272HCID 14127272、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
25 °C

実験手順

A solution of 3.0 g of (1S,6R)-8,8-dichlorobicyclo [4.2.0]oct-2-en-7-one, the compound of formula (4), is dissolved in 120 ml of methanol and treated at 0° C. with 1.2 g of sodium borohydride, and the mixture is stirred at 25° C. for 1 hour. The solvent is removed under reduced pressure and the residue partitioned between methylene chloride and water. The extract is dried over anhydrous sodium sulfate, filtered and the solvent removed under reduced pressure. The residue is recrystallized from hexane to give (1S,6R,7R)-8,8-dichlorobicyclo[4.2.0]oct-2-en-7-ol, [α]D =+214.4° (CHCl3).

後処理

  1. customThe solvent is removed under reduced pressure
  2. customthe residue partitioned between methylene chloride and water
  3. dry with materialThe extract is dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. customthe solvent removed under reduced pressure
  6. customThe residue is recrystallized from hexane

出典と根拠

ORDレコード
ord-dac26307a020400b9acdce72bb4f5354
出典データセット
uspto-grants-1991_09
特許番号
US05049497

反応ノート

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