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Phosphoric Acid → (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one monophosphate

HRID 1875698
ノート
印刷プレビュー

反応式

HRID 1875698 の反応式
[OH:1][CH2:2][C@H:3]1[CH2:7][CH2:6][CH2:5][N:4]1[CH2:8][CH2:9][C:10]1[NH:11][C:12](=[O:21])[C:13]2[C:18]([CH:19]=1)=[C:17]([CH3:20])[CH:16]=[CH:15][CH:14]=2.[P:22](=[O:26])([OH:25])([OH:24])[OH:23]>C(O)C>[P:22]([OH:26])([OH:25])([OH:24])=[O:23].[OH:1][CH2:2][C@H:3]1[CH2:7][CH2:6][CH2:5][N:4]1[CH2:8][CH2:9][C:10]1[NH:11][C:12](=[O:21])[C:13]2[C:18]([CH:19]=1)=[C:17]([CH3:20])[CH:16]=[CH:15][CH:14]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 1004Phosphoric AcidHCID 10424118(R)-3-(2-(2-(hydroxymethyl)pyrrolidin-1-yl)ethyl)-5-methylisoquinolin-1(2H)-one

生成物 1

HCID 25164152(R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one monophosphate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A free form (1 g) of (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one was measured, ethanol (40 ml) was added and the mixture was completely dissolved by heating under reflux. Thereto was added commercially available 85% phosphoric acid (200 μL) and the mixture was left stirring at room temperature for 1 hr. The precipitate was collected by filtration and dissolved again in water (1 mL) at 80° C. Ethanol (8 mL) was added and the mixture was left standing at room temperature for 1 hr. The resulting precipitate was collected by filtration and dried under reduced pressure at 50° C. for 9 hr to give the title compound (838 mg).

後処理

  1. dissolutionthe mixture was completely dissolved
  2. temperatureby heating
  3. temperatureunder reflux
  4. waitthe mixture was left
  5. filtrationThe precipitate was collected by filtration
  6. dissolutiondissolved again in water (1 mL) at 80° C
  7. additionEthanol (8 mL) was added
  8. waitthe mixture was left
  9. waitstanding at room temperature for 1 hr
  10. filtrationThe resulting precipitate was collected by filtration
  11. customdried under reduced pressure at 50° C. for 9 hr

出典と根拠

ORDレコード
ord-d71089bce50045149252bd98143cd3b0
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08309573B2

反応ノート

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