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Sodium Bicarbonate → 1-(3-Benzo[1,3]dioxol-5-ylmethylpiperazin-1-yl)-7-methoxyisoquinoline

HRID 1714806
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HRID 1714806 반응식
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]3[CH2:16][N:15]([C:17]4[C:26]5[C:21](=[CH:22][CH:23]=[C:24]([O:27][CH3:28])[CH:25]=5)[CH:20]=[CH:19][N:18]=4)[CH2:14][CH2:13][N:12]3C(OC(C)(C)C)=O)=[CH:9][C:4]=2[O:3][CH2:2]1.C(=O)([O-])O.[Na+]>Cl.O1CCOCC1>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]3[NH:12][CH2:13][CH2:14][N:15]([C:17]4[C:26]5[C:21](=[CH:22][CH:23]=[C:24]([O:27][CH3:28])[CH:25]=5)[CH:20]=[CH:19][N:18]=4)[CH2:16]3)=[CH:9][C:4]=2[O:3][CH2:2]1
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참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 231558011-(2-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazin-4-yl)-7-methoxyisoquinoline

생성물 1

HCID 231557261-(3-Benzo[1,3]dioxol-5-ylmethylpiperazin-1-yl)-7-methoxyisoquinoline수율 58.2%

시약·촉매·용매 1

HCID 204431481,4-Dioxane hydrochloride용매

실험 절차

In 10 ml of 4N hydrochloric acid-dioxane solution, 150 mg of 1-(2-benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazin-4-yl)-7-methoxyisoquinoline as synthesized in the above step was added and stirred for 18 hours. The solution was neutralized with saturated aqueous sodium hydrogencarbonate solution, extracted with ethyl acetate, dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified on silica gel column chromatography (methanol:chloroform=1:9) to provide 69 mg (58%) of 1-(3-benzo[1,3]dioxol-5-ylmethylpiperazin-1-yl)-7-methoxyisoquinoline.

후처리

  1. additionwas added
  2. extractionextracted with ethyl acetate
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was purified on silica gel column chromatography (methanol:chloroform=1:9)

출처 및 근거

ORD 기록
ord-fc517de01535461d928992a7e2a5de0e
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07799775B2

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