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Water → 1-(2-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazin-4-yl)-7-methoxyisoquinoline

HRID 1714805
ノート
印刷プレビュー

反応式

HRID 1714805 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]3[CH2:16][NH:15][CH2:14][CH2:13][N:12]3[C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])=[CH:9][C:4]=2[O:3][CH2:2]1.Cl[C:25]1[C:34]2[C:29](=[CH:30][CH:31]=[C:32]([O:35][CH3:36])[CH:33]=2)[CH:28]=[CH:27][N:26]=1.C(N(CC)CC)C.O>C(O)CO>[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]3[CH2:16][N:15]([C:25]4[C:34]5[C:29](=[CH:30][CH:31]=[C:32]([O:35][CH3:36])[CH:33]=5)[CH:28]=[CH:27][N:26]=4)[CH2:14][CH2:13][N:12]3[C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])=[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

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 222501811-Chloro-7-methoxyisoquinolineHCID 231556182-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazine

生成物 1

HCID 231558011-(2-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazin-4-yl)-7-methoxyisoquinoline収率 44%

試薬・触媒・溶媒 1

HCID 174
Ethylene Glycol
溶媒

実験手順

A mixture of 320 mg of 2-benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazine as synthesized in the above step, 200 mg of 1-chloro-7-methoxyisoquinoline and 100 mg of triethylamine was stirred in 2 ml of ethylene glycol at 150° C. for 18 hours. After addition of water, the solution was 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 (ethyl acetate:n-hexane=1:1) to provide 210 mg (44%) of 1-(2-benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazin-4-yl)-7-methoxyisoquinoline.

後処理

  1. extractionthe solution was extracted with ethyl acetate
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified on silica gel column chromatography (ethyl acetate:n-hexane=1:1)

出典と根拠

ORDレコード
ord-89884b65e752497cbe03964188c7a8bd
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

読み込み中…

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