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Methanol → alpha-(3,4-Dimethoxy-benzal)-beta-methoxy-propionitrile

HRID 2351307
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HRID 2351307 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH:6]=O.[CH3:13][O:14][CH2:15][CH2:16][C:17]#[N:18].CO.[OH-].[K+]>O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][C:10]=1[O:11][CH3:12])[CH:6]=[C:16]([CH2:15][O:14][CH3:13])[C:17]#[N:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 8419VeratraldehydeHCID 14797Potassium Hydroxide2회HCID 61032Propanenitrile, 3-methoxy-

생성물 1

HCID 111305alpha-(3,4-Dimethoxy-benzal)-beta-methoxy-propionitrile수율 100%

시약·촉매·용매 1

HCID 962Water용매

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온도
30 °C

실험 절차

A mixture of 200 g (1.20 mole) of 3,4-dimethoxy-benzaldehyde, 150 g (1.75 mole) of β-methoxy-propinitrile, 260 ml of methanol and 10 g of a 55% methanolic potassium hydroxide solution is stirred at 60°-62° C. for 8 hours, whereupon the reaction mixture is cooled to 30° C., and 170 g of a 55% methanolic potassium hydroxide solution are added dropwise. The reaction mixture is stirred for 5 hours and diluted with 1000 ml of water. The precipitated crystalline product is filtered, washed with methanol and water. Thus 280 g of α-(3,4-dimethoxy-benzal)-β-methoxy-propionitrile are obtained, yield 85%, mp.: 82°-83° C.

후처리

  1. stirringThe reaction mixture is stirred for 5 hours
  2. filtrationThe precipitated crystalline product is filtered
  3. washwashed with methanol and water

출처 및 근거

ORD 기록
ord-ef0842d94a3849718e1bcac0753f13a2
출처 데이터셋
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04873249

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