Sodium ethoxide → 3-Ethoxymethylisoquinoline

HRID 443811

반응식

HRID 443811 반응식
Cl.Cl[CH2:3][C:4]1[N:5]=[CH:6][C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][CH:8]=2.[O-:14][CH2:15][CH3:16].[Na+]>C(O)C>[CH2:15]([O:14][CH2:3][C:4]1[N:5]=[CH:6][C:7]2[C:12]([CH:13]=1)=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH3:16]

참가 물질

4

반응물 2

HCID 2723922Sodium ethoxideHCID 128748713-(Chloromethyl)isoquinoline hydrochloride

생성물 1

HCID 128748433-Ethoxymethylisoquinoline수율 88.6%

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
20 °C

실험 절차

A mixture of 3-chloromethylisoquinoline hydrochloride (40 g) and sodium ethoxide (40 g) in ethanol (700 cc) is heated under reflux for 8 hours. After cooling to 20° C., the mixture is filtered and the filtrate is evaporated to dryness at 50° C. under reduced pressure (20 mm Hg). The residue is taken up in methylene chloride (500 cc), the mixture is washed with water (3×100 cc), the organic phase is dried over magnesium sulphate and filtered and the filtrate is evaporated to dryness at 40° C. under reduced pressure (20 mm Hg). The oily residue is distilled at 110°-114° C. under a pressure of 0.6 mm Hg. 3-Ethoxymethylisoquinoline (31 g), a colourless oil, is obtained.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 8 hours
  3. filtrationthe mixture is filtered
  4. customthe filtrate is evaporated to dryness at 50° C. under reduced pressure (20 mm Hg)
  5. washthe mixture is washed with water (3×100 cc)
  6. dry with materialthe organic phase is dried over magnesium sulphate
  7. filtrationfiltered
  8. customthe filtrate is evaporated to dryness at 40° C. under reduced pressure (20 mm Hg)
  9. distillationThe oily residue is distilled at 110°-114° C. under a pressure of 0.6 mm Hg

출처 및 근거

ORD 기록
ord-e1a391845c2d43eeb4c5a2a412c44c74
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04261993

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