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

HRID 8719

반응식

HRID 8719 반응식
[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

참가 물질

5

반응물 1

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

생성물 1

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

시약·촉매·용매 3

HCID 345198Adams' catalyst촉매HCID 313Hydrochloric Acid용매HCID 887Methanol용매

실험 절차

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 11a as a pale yellow foam. The crude hydrochloride salt of the product was used in the next step without further purification.

후처리

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

출처 및 근거

ORD 기록
ord-e40ebc98c10d4b63a935db49375dcd88
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091200B2

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