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 Carbonate → 1-(4-Ethynyl-3-methoxyphenyl)-4-methylpiperazine

HRID 1403209
ノート
印刷プレビュー

反応式

HRID 1403209 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:15]2[CH2:20][CH2:19][N:18]([CH3:21])[CH2:17][CH2:16]2)[CH:6]=[CH:7][C:8]=1[C:9]#[C:10][Si](C)(C)C.C(=O)([O-])[O-].[K+].[K+]>CO>[C:9]([C:8]1[CH:7]=[CH:6][C:5]([N:15]2[CH2:16][CH2:17][N:18]([CH3:21])[CH2:19][CH2:20]2)=[CH:4][C:3]=1[O:2][CH3:1])#[CH:10]
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 11430Potassium CarbonateHCID 867252923-Methoxy-4-[(trimethylsilyl)ethynyl]phenyl-4-methylpiperazine

生成物 1

HCID 712395881-(4-Ethynyl-3-methoxyphenyl)-4-methylpiperazine収率 84.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 1-{3-methoxy-4-[(trimethylsilyl)ethynyl]phenyl-4-methylpiperazine (583 mg, 1.927 mmol) in anhydrous methanol (12 mL) is treated with powdered anhydrous potassium carbonate under stirring at room temperature for 1.5 h. After removing the solvent under vacuum the residue was taken up with EtOAc (80 mL) and water (5 mL). The phases were separated, the organic phase was washed with brine (3×10 mL), water (10 mL), dried over sodium sulfate and the solvent removed under vacuum. The dark oil obtained was purified by chromatography on silica gel (DCM/MeOH/TEA 90/10/0.1) to give the title compound as brownish solid (374 mg, 84.2%).

後処理

  1. customAfter removing the solvent under vacuum the residue
  2. customThe phases were separated
  3. washthe organic phase was washed with brine (3×10 mL), water (10 mL)
  4. dry with materialdried over sodium sulfate
  5. customthe solvent removed under vacuum
  6. customThe dark oil obtained
  7. customwas purified by chromatography on silica gel (DCM/MeOH/TEA 90/10/0.1)

出典と根拠

ORDレコード
ord-a062148cf68948158b9cfee5bdb75259
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08912200B2

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