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(R)-3-(2-(2-(hydroxymethyl)pyrrolidin-1-yl)ethyl)-5-methylisoquinolin-1(2H)-one → (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one monomesylate

HRID 1875701
ノート
印刷プレビュー

反応式

HRID 1875701 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.C(O)C.[CH3:25][S:26]([OH:29])(=[O:28])=[O:27]>C(O)C>[S:26]([OH:29])(=[O:28])(=[O:27])[CH3:25].[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
参加物反応条件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 10424118(R)-3-(2-(2-(hydroxymethyl)pyrrolidin-1-yl)ethyl)-5-methylisoquinolin-1(2H)-oneHCID 86653870Methanesulfonic acid ethanol

生成物 1

HCID 86653869(R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one monomesylate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
50 °C

実験手順

To a solution (4 mL) of a free form (500 mg) of (R)-3-[2-(2-hydroxymethylpyrrolidin-1-yl)ethyl]-5-methyl-2H-isoquinolin-1-one in ethanol was added dropwise 2M methanesulfonic acid ethanol solution (1 mL) with stirring on an oil bath at 50° C. The bath was removed, ethyl acetate (8 mL) and seed crystals were added and the mixture was stirred to allow precipitation of crystals. After stirring under ice-cooling, the crystals were collected through filtration, washed with ethyl acetate/ethanol (2:1) and dried under reduced pressure at 50° C. for 18 hr to give the title compound (507 mg).

後処理

  1. customThe bath was removed
  2. additionethyl acetate (8 mL) and seed crystals were added
  3. stirringthe mixture was stirred
  4. customprecipitation of crystals
  5. stirringAfter stirring under ice-
  6. temperaturecooling
  7. filtrationthe crystals were collected through filtration
  8. washwashed with ethyl acetate/ethanol (2:1)
  9. customdried under reduced pressure at 50° C. for 18 hr

出典と根拠

ORDレコード
ord-a691628029ff4edab309d6149433347e
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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