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

HRID 1653663ノート

反応式

HRID 1653663 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.).

後処理

  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.)

出典と根拠

ORDレコード
ord-2117492620c64e508d70bf691f2e13f7
出典データセット
uspto-grants-1995_04
特許番号
US05403839

反応ノート

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