ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Potassium Hydroxide → 2-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazine

HRID 1714804
ノート
印刷プレビュー

反応式

HRID 1714804 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([CH2:10][CH:11]3[C:16](=O)[NH:15][CH2:14][CH2:13][N:12]3[C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[CH:9][C:4]=2[O:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[K+]>O1CCCC1>[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:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])=[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

5

反応物 3

HCID 14797Potassium HydroxideHCID 21226445Aluminium lithium hydrideHCID 231559092-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonyl-3-oxopiperazine

生成物 1

HCID 231556182-Benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazine収率 66.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Dissolving 2.00 g of 2-benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonyl-3-oxopiperazine as synthesized in the above step in 50 ml of tetrahydrofuran, 1.00 g of lithium aluminium hydride was added to the solution which then was heated under reflux for 16 hours. To the solution 10% aqueous potassium hydroxide solution was added, the insoluble matter was filtered off, extracted with ethyl acetate, the extract was 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=1:19) to provide 1.27 g (66%) of 2-benzo[1,3]dioxol-5-ylmethyl-1-tert-butoxycarbonylpiperazine.

後処理

  1. temperaturethen was heated
  2. temperatureunder reflux for 16 hours
  3. filtrationthe insoluble matter was filtered off
  4. extractionextracted with ethyl acetate
  5. dry with materialthe extract was dried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified on silica gel column chromatography (methanol:chloroform=1:19)

出典と根拠

ORDレコード
ord-30d5f4a6f16e45f4873d184662d36bc2
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…

このページの内容参加物実験手順後処理出典と根拠反応ノート