Water → 3,6-Dimethyl-2,4-heptanediol

HRID 132739

反応式

HRID 132739 の反応式
[BH4-].[Na+].[OH-].[Na+].O.[CH3:6][CH:7]([C:11](=[O:16])[CH2:12][CH:13]([CH3:15])[CH3:14])[C:8](=[O:10])[CH3:9]>CO>[CH3:6][CH:7]([CH:11]([OH:16])[CH2:12][CH:13]([CH3:15])[CH3:14])[CH:8]([OH:10])[CH3:9]

参加物

6

反応物 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 5382833,6-Dimethylheptane-2,4-dioneHCID 4311764Sodium borohydride

生成物 1

HCID 671601493,6-Dimethyl-2,4-heptanediol収率 90%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To the mixture of 2.5 g sodium borohydride, 0.05 g sodium hydroxide, and 25 ml water was added dropwise the mixture of 14.2 g 3,6-dimethyl-2,4-heptandione and 30 ml methanol at 0-10° C. Upon completing the addition, the solvent was removed by reduced pressure distillation. The reaction mixture was continuously extracted with 40 ml ethyl acetate for 15 hours. The solvent was removed. Distillation under reduced pressure gave colorless liquid 3,6-dimethyl-2,4-heptanediol, and the yield was 90%. IR spectrum had a strong absorption peak at 3400 cm−1, and had no absorption peak at about 1700 cm−1. This demonstrated that the reduction reaction was carried out completely.

後処理

  1. additionwas added dropwise
  2. additionthe addition
  3. customthe solvent was removed by reduced pressure distillation
  4. extractionThe reaction mixture was continuously extracted with 40 ml ethyl acetate for 15 hours
  5. customThe solvent was removed
  6. distillationDistillation under reduced pressure

出典と根拠

ORDレコード
ord-d687d064df1b462b9f2cce4640fe904f
出典データセット
uspto-grants-2008_06
特許番号
US07388061B2

関連ノート

読み込み中…