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Benzaldehyde → 2-(Dimethoxymethyl)-3-phenylacrylonitrile

HRID 496819
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HRID 496819 반응식
[CH:1](=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:9][O:10][CH:11]([O:15][CH3:16])[CH2:12][C:13]#[N:14].C[O-].[Na+]>CO>[CH3:9][O:10][CH:11]([O:15][CH3:16])[C:12](=[CH:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[C:13]#[N:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 240BenzaldehydeHCID 937313,3-DimethoxypropiononitrileHCID 10942334Sodium Methoxide

생성물 1

HCID 538099012-(Dimethoxymethyl)-3-phenylacrylonitrile수율 68%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Benzaldehyde (79.5 g, 0.75 mol) and 3,3-dimethoxypropionitrile (115.1 g, 1.0 mol) were mixed together and added to a solution of sodium methoxide (54.0 g, 1.0 mol) in methanol (400 mL) over a period of 15 minutes. The mixture was stirred at room temperature overnight. Most of the methanol was evaporated in vacuo and the residue was partitioned between ethyl acetate (500 mL) and water (450 mL). The organic layer was separated, washed with brine (400 mL), dried (MgSO4) and the solvent evaporated in vacuo. The residual oil was distilled to give 103 g (68%) of the product as a colorless oil, bp 125-130° C. (2 mm Hg).

후처리

  1. customMost of the methanol was evaporated in vacuo
  2. customthe residue was partitioned between ethyl acetate (500 mL) and water (450 mL)
  3. customThe organic layer was separated
  4. washwashed with brine (400 mL)
  5. dry with materialdried (MgSO4)
  6. customthe solvent evaporated in vacuo
  7. distillationThe residual oil was distilled

출처 및 근거

ORD 기록
ord-2dbbaa9df03f4353865da47aa9bc6ae9
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06946554B2

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