Hydrochloric Acid → Ethyl 6H-pyrido[3,2,1-de]acridin-1(2H)-one

HRID 54923노트

반응식

HRID 54923 반응식
[O-][CH2:2][CH3:3].[Na+].[C:5]1(=[O:22])[N:20]2[C:21]3[C:12](=[CH:13][C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][C:19]=42)[CH2:11][CH:10]=[CH:9][C:8]=3[CH2:7][CH2:6]1.C(=O)(OCC)OCC.Cl>C(O)C>[CH2:2]([CH:6]1[C:5](=[O:22])[N:20]2[C:21]3[C:12](=[CH:13][C:14]4[CH:15]=[CH:16][CH:17]=[CH:18][C:19]=42)[CH2:11][CH:10]=[CH:9][C:8]=3[CH2:7]1)[CH3:3]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7766Diethyl CarbonateHCID 2723922Sodium ethoxideHCID 677259016H-pyrido[3,2,1-de]acridin-1(2H)-one

생성물 1

HCID 67724926Ethyl 6H-pyrido[3,2,1-de]acridin-1(2H)-one

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a freshly prepared solution of sodium ethoxide in ethanol (from 0.35 g sodium metal and 10 ml ethanol) was added 6H-pyrido[3,2,1-de]acridin-1(2H)-one (1.2 g) portionwise over a period of 10 minutes. To the resulting dark red solution was slowly added diethyl carbonate (1.77 g) and the solution was then refluxed for 3 hours. The reaction mixture was cooled, acidified to pH 2 with concentrated HCl and then extracted with methylene chloride. The organic extract was washed with water and was then collected, dried and evaporated to dryness to obtain a light amber solid (1.8 g; m.p. 113°-118° C.).

후처리

  1. temperaturethe solution was then refluxed for 3 hours
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with methylene chloride
  4. extractionThe organic extract
  5. washwas washed with water
  6. customwas then collected
  7. customdried
  8. customevaporated to dryness
  9. customto obtain a light amber solid (1.8 g; m.p. 113°-118° C.)

출처 및 근거

ORD 기록
ord-e0d857e89cd04585803ccfc2a77737d0
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624929

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