Sodium Bisulfite → Hydroxy-[4-(4-isopropyl-piperazine-1-carbonyl)-phenyl]-methanesulfonic acid sodium salt

HRID 13545

反応式

HRID 13545 の反応式
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:19]=[CH:18][C:15]([CH:16]=[O:17])=[CH:14][CH:13]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[OH:20][S:21]([O-:23])=[O:22].[Na+:24]>CCO.O>[Na+:24].[OH:17][CH:16]([C:15]1[CH:14]=[CH:13][C:12]([C:10]([N:7]2[CH2:8][CH2:9][N:4]([CH:1]([CH3:3])[CH3:2])[CH2:5][CH2:6]2)=[O:11])=[CH:19][CH:18]=1)[S:21]([O-:23])(=[O:22])=[O:20]

参加物

5

反応物 2

HCID 23665763Sodium BisulfiteHCID 574785811-(4-Formylbenzoyl)-4-isopropylpiperazine

生成物 1

HCID 59340029Hydroxy-[4-(4-isopropyl-piperazine-1-carbonyl)-phenyl]-methanesulfonic acid sodium salt

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

A solution of 4-(4-isopropyl-piperazine-1-carbonyl)-benzaldehyde (20.0 g, 76.9 mmol) in EtOH (200 mL) was stirred at room temperature for 15 min. To the resulting solution was added a solution of NaHSO3 (9.6 g) in H2O (25 mL), dropwise over 30 min. The resulting suspension was stirred at room temperature for 2 h, then cooled to 0° C. and stirred for 3 h, adding EtOH periodically (total 200 mL) to aid stirring. A precipitate formed and was collected by suction filtration through a glass frit lined with filter paper. The filter cake was washed with hexane (1×50 mL), and dried under vacuum for 16 h to yield the title compound as a white solid.

後処理

  1. temperaturecooled to 0° C.
  2. stirringstirred for 3 h
  3. stirringto aid stirring
  4. customA precipitate formed
  5. filtrationwas collected by suction filtration through a glass frit
  6. filtrationwith filter paper
  7. washThe filter cake was washed with hexane (1×50 mL)
  8. customdried under vacuum for 16 h

出典と根拠

ORDレコード
ord-4a9435fcea3d419e8d97eb77a8f43fff
出典データセット
uspto-grants-2010_06
特許番号
US07728129B2

関連ノート

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