Hydrochloric Acid → 1-[1-(4-Pyridyl)-4-piperidinylamino]-2-piperazinone trihydrochloride

HRID 2086235ノート

反応式

HRID 2086235 の反応式
C(OC([N:11]1[CH2:16][CH2:15][N:14]([NH:17][CH:18]2[CH2:23][CH2:22][N:21]([C:24]3[CH:29]=[CH:28][N:27]=[CH:26][CH:25]=3)[CH2:20][CH2:19]2)[C:13](=[O:30])[CH2:12]1)=O)C1C=CC=CC=1.[ClH:31]>C(OCC)(=O)C.CO.[Pd]>[ClH:31].[ClH:31].[ClH:31].[N:27]1[CH:28]=[CH:29][C:24]([N:21]2[CH2:20][CH2:19][CH:18]([NH:17][N:14]3[CH2:15][CH2:16][NH:11][CH2:12][C:13]3=[O:30])[CH2:23][CH2:22]2)=[CH:25][CH:26]=1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 178254544-Benzyloxycarbonyl-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone

生成物 1

HCID 695456121-[1-(4-Pyridyl)-4-piperidinylamino]-2-piperazinone trihydrochloride

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 4-benzyloxycarbonyl-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone (25.29 g) and an a 4N solution of hydrochloric acid in ethyl acetate (15.5 ml) in methanol (300 ml) was combined with 10% Pd/C (50% hydrated, 5.00 g) and stirred at room temperature for 15 hours under a hydrogen atmosphere. The catalyst was filtered off, and the reaction mixture was concentrated. The residue was dissolved in ethanol (300 ml), and combined with a 4N solution of hydrochloric acid in ethyl acetate (31 ml). The crystals precipitated were collected by filtration and dried to obtain 1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone trihydrochloride (20.16 g) as colorless crystals.

後処理

  1. filtrationThe catalyst was filtered off
  2. concentrationthe reaction mixture was concentrated
  3. dissolutionThe residue was dissolved in ethanol (300 ml)
  4. customThe crystals precipitated
  5. filtrationwere collected by filtration
  6. customdried

出典と根拠

ORDレコード
ord-0d55b9eb262941a982003bef791d5c1f
出典データセット
uspto-grants-2004_04
特許番号
US06723722B1

反応ノート

読み込み中…