Piperazine, 1-(5-isoquinolinylsulfonyl)-4-methyl- → 5-(4-Methyl-piperazine-1-sulfonyl)-1,2,3,4-tetrahydro-isoquinoline

HRID 2183703

反応式

HRID 2183703 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([S:8]([C:11]2[CH:20]=[CH:19][CH:18]=[C:17]3[C:12]=2[CH:13]=[CH:14][N:15]=[CH:16]3)(=[O:10])=[O:9])[CH2:4][CH2:3]1>Cl.CO.O=[Pt]=O>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([S:8]([C:11]2[CH:20]=[CH:19][CH:18]=[C:17]3[C:12]=2[CH2:13][CH2:14][NH:15][CH2:16]3)(=[O:9])=[O:10])[CH2:4][CH2:3]1

参加物

5

反応物 1

HCID 13116934Piperazine, 1-(5-isoquinolinylsulfonyl)-4-methyl-

生成物 1

HCID 219836535-(4-Methyl-piperazine-1-sulfonyl)-1,2,3,4-tetrahydro-isoquinoline収率 124.1%

試薬・触媒・溶媒 3

HCID 345198Adams' catalyst触媒HCID 313Hydrochloric Acid溶媒HCID 887Methanol溶媒

実験手順

5-(4-Methyl-piperazine-1-sulfonyl)-isoquinoline 10a (0.99 g, 3.41 mmol) was dissolved in a solution 2% of HCl in methanol (100 mL) under nitrogen. PtO2 (250 mg) was added under nitrogen and the mixture was hydrogenated in a Parr apparatus at 45 psi for 3.5 h. The catalyst was removed by filtration, rinsed with MeOH, and the filtrate was concentrated in vacuo to give 1.25 g of 5-(4-methyl-piperazine-1-sulfonyl)-1,2,3,4-tetrahydro-isoquinoline 11 a as a pale yellow foam. The crude hydrochloride salt of the product was used in the next step without further purification.

後処理

  1. customThe catalyst was removed by filtration
  2. washrinsed with MeOH
  3. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-bf54838716374703bdd9c803a88a5c4b
出典データセット
uspto-grants-2005_05
特許番号
US06900220B2

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