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

HRID 2183703

반응식

HRID 2183703 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 11 a 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-bf54838716374703bdd9c803a88a5c4b
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06900220B2

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