Acetone → SAR-407899 hydrochloride dihydrate

HRID 2370256ノート

反応式

HRID 2370256 の反応式
[ClH:1].[NH:2]1[CH2:7][CH2:6][CH:5]([O:8][C:9]2[CH:10]=[C:11]3[C:16](=[CH:17][CH:18]=2)[C:15](=[O:19])[NH:14][CH:13]=[CH:12]3)[CH2:4][CH2:3]1.CC(C)=[O:22]>O>[OH2:8].[OH2:22].[ClH:1].[NH:2]1[CH2:3][CH2:4][CH:5]([O:8][C:9]2[CH:10]=[C:11]3[C:16](=[CH:17][CH:18]=2)[C:15](=[O:19])[NH:14][CH:13]=[CH:12]3)[CH2:6][CH2:7]1

参加物

4

反応物 2

HCID 180AcetoneHCID 426359186-[(Piperidin-4-yl)oxy]isoquinolin-1(2H)-one--hydrogen chloride (1/1)

生成物 1

HCID 86675574SAR-407899 hydrochloride dihydrate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

8.5 g of crude 6-(Piperidin-4-yloxy)-2H-isoquinolin-1-one hydrochloride were dissolved in 21.5 mL water at 65° C. The temperature was lowered to 50° C. in 1 h and 32.3 mL acetone were added in 30 min. The temperature was lowered to 40° C. and the mixture was stirred for 3 h. The reaction mixture was chilled to ambient temperature. The crystalline material was collected, washed with water/acetone (1/3) and dried to yield 4.54 g (purity>99.9%) of 6-(Piperidin-4-yloxy)-2H-isoquinolin-1-one hydrochloride dihydrate.

後処理

  1. customwas lowered to 40° C.
  2. customThe crystalline material was collected
  3. washwashed with water/acetone (1/3)
  4. customdried

出典と根拠

ORDレコード
ord-86f3b20ea37d4f45802dbb1fadcba9a6
出典データセット
uspto-grants-2014_04
特許番号
US08710078B2

反応ノート

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