Sodium Sulfate → 2,2-diethoxypropan-1-ol

HRID 1271800ノート

反応式

HRID 1271800 の反応式
[CH2:1]([O:3][C:4]([O:11][CH2:12][CH3:13])([CH3:10])[C:5](OCC)=[O:6])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].S([O-])([O-])(=O)=O.[Na+].[Na+]>C(OCC)C>[CH2:1]([O:3][C:4]([O:11][CH2:12][CH3:13])([CH3:10])[CH2:5][OH:6])[CH3:2]

参加物

5

反応物 3

HCID 24436Sodium SulfateHCID 95835Ethyl 2,2-diethoxypropionateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 117010602,2-diethoxypropan-1-ol収率 76.3%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

A solution of ethyl pyruvate diethyl ketal (16.0 g, 0.084 moles) in ethyl ether (60 mL) was added dropwise during 30 min to a stirred solution of lithium aluminum hydride (1.90 g, 0.050 moles) in ethyl ether (150 mL). Next the mixture was stirred 1 h at room temperature under nitrogen atmosphere. Saturated solution of sodium sulfate (20 mL) was added and the mixture was stirred 15 min. Next the mixture was filtered, dried with anhydrous magnesium sulfate, and the solvent was distilled off. The residue was subjected to fractional vacuum distillation giving 9.5 g of pure 2,2-diethoxypropan-1-ol. NMR (d6-DMSO): 1.17 ppm (t, —CH3, ethyl (ketal), 6H), 1.31 ppm (s, —CH3—C—CH2OH, 3H), 3.37 ppm (q, —OCH2CH3, (ketal), 4H), 3.86 ppm (d, —CH2OH, 2H), 4.45 ppm (t, —OH, 1H).

後処理

  1. stirringthe mixture was stirred 15 min
  2. filtrationNext the mixture was filtered
  3. dry with materialdried with anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off
  5. distillationThe residue was subjected to fractional vacuum distillation

出典と根拠

ORDレコード
ord-c0819d9a097d4390b2423468d5268f55
出典データセット
uspto-grants-2007_04
特許番号
US07208145B2

反応ノート

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