2-Acetyl-5-methylthiophene → 1-(5-Methyl-2-thienyl)ethanol

HRID 2041236

反応式

HRID 2041236 の反応式
[BH4-].[Na+].[C:3]([C:6]1[S:7][C:8]([CH3:11])=[CH:9][CH:10]=1)(=[O:5])[CH3:4]>CO>[OH:5][CH:3]([C:6]1[S:7][C:8]([CH3:11])=[CH:9][CH:10]=1)[CH3:4]

参加物

4

反応物 2

HCID 836552-Acetyl-5-methylthiopheneHCID 4311764Sodium borohydride

生成物 1

HCID 150917951-(5-Methyl-2-thienyl)ethanol収率 98.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Add sodium borohydride (270 mg, 7.13 mmol) to a solution of 2-acetyl-5-methylthiophene (1.0 g, 7.13 mmol) in methanol (40 mL). Stir the mixture for 1 h at room temperature. Remove the solvent in vacuo and partition the residue between water and DCM. Separate the organic phase, dry over Na2SO4, filter and concentrate to obtain the desired intermediate as an oil (0.995 g, 98%) that was used without further purification. GC-MS m/z 142 (M+).

後処理

  1. customRemove the solvent in vacuo
  2. custompartition the residue between water and DCM
  3. customSeparate the organic phase
  4. dry with materialdry over Na2SO4
  5. filtrationfilter
  6. concentrationconcentrate

出典と根拠

ORDレコード
ord-ed1bacafb5dc48c49f16aff7d56c8e5b
出典データセット
uspto-grants-2013_11
特許番号
US08580780B2

関連ノート

読み込み中…