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

HRID 1714806
ノート
印刷プレビュー

反応式

HRID 1714806 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 204431481,4-Dioxane hydrochloride溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-fc517de01535461d928992a7e2a5de0e
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07799775B2

反応ノート

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