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

HRID 537649노트

반응식

HRID 537649 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 117010602,2-diethoxypropan-1-ol수율 76.3%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6e36eb88216f4ce7a65a4a550bf39111
출처 데이터셋
uspto-grants-2014_10
특허 번호
US08865149B2

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