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Sodium Hydroxide → (R)-3-(2-(2-(hydroxymethyl)pyrrolidin-1-yl)ethyl)-5-methylisoquinolin-1(2H)-one

HRID 2373281
ノート
印刷プレビュー

反応式

HRID 2373281 の反応式
Cl.[OH:2][CH2:3][C@H:4]1[CH2:8][CH2:7][CH2:6][N:5]1[CH2:9][CH2:10][C:11]1[O:12][C:13]([C:15]2[C:20]([CH:21]=1)=[C:19]([CH3:22])[CH:18]=[CH:17][CH:16]=2)=O.C(=O)([O-])[O-].[NH4+:27].[NH4+].[OH-].[Na+]>C(O)(=O)C>[OH:2][CH2:3][C@H:4]1[CH2:8][CH2:7][CH2:6][N:5]1[CH2:9][CH2:10][C:11]1[NH:27][C:13](=[O:12])[C:15]2[C:20]([CH:21]=1)=[C:19]([CH3:22])[CH:18]=[CH:17][CH:16]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 517111Ammonium CarbonateHCID 68644204(R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methylisocoumarin hydrochloride

生成物 1

HCID 10424118(R)-3-(2-(2-(hydroxymethyl)pyrrolidin-1-yl)ethyl)-5-methylisoquinolin-1(2H)-one収率 75.7%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

(R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methylisocoumarin hydrochloride (62 g) and acetic acid (186 mL) were added and ammonium carbonate (74.4 g) was gradually added to the mixture with stirring. After bubbling, the reaction mixture was heated and stirred at 130° C. for 2 hr with heating. After the completion of the reaction, the reaction mixture was cooled to room temperature and aqueous sodium hydroxide (140 g) solution (200 mL) was added. The mixture was stirred at 80° C., and after the completion of the reaction, the reaction mixture was concentrated. The methanol fraction was evaporated and the mixture was extracted twice with chloroform. The organic layer was extracted twice with 3N hydrochloric acid (300 mL and 100 mL), and potassium carbonate was added to the aqueous layer to basify the layer. The aqueous layer was extracted twice with chloroform, and the extract was dried over magnesium sulfate. The solvent was concentrated and ethyl acetate was added to the obtained residue. The mixture was further concentrated and the residue was dissolved in a small amount of ethyl acetate with heating. Diethyl ether was added to the solution and the precipitated crystals were collected by filtration to give (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one (41.5 g).

後処理

  1. customAfter bubbling
  2. temperaturethe reaction mixture was heated
  3. stirringstirred at 130° C. for 2 hr
  4. temperaturewith heating
  5. customAfter the completion of the reaction
  6. stirringThe mixture was stirred at 80° C.
  7. customafter the completion of the reaction
  8. concentrationthe reaction mixture was concentrated
  9. customThe methanol fraction was evaporated
  10. extractionthe mixture was extracted twice with chloroform
  11. extractionThe organic layer was extracted twice with 3N hydrochloric acid (300 mL and 100 mL), and potassium carbonate
  12. additionwas added to the aqueous layer
  13. extractionThe aqueous layer was extracted twice with chloroform
  14. dry with materialthe extract was dried over magnesium sulfate
  15. concentrationThe solvent was concentrated
  16. additionethyl acetate was added to the obtained residue
  17. concentrationThe mixture was further concentrated
  18. dissolutionthe residue was dissolved in a small amount of ethyl acetate
  19. temperaturewith heating
  20. additionDiethyl ether was added to the solution
  21. filtrationthe precipitated crystals were collected by filtration

出典と根拠

ORDレコード
ord-636cf8c24d5f47c0abc48e9995a902e6
出典データセット
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07459465B2

反応ノート

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