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

Diisobutylaluminum hydride → 2-(1-(4-Chloro-3-methoxyphenyl)piperidin-4-ylidene)ethanol

HRID 1804854
ノート
印刷プレビュー

反応式

HRID 1804854 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:13][CH2:12][C:11](=[CH:14][C:15](OC)=[O:16])[CH2:10][CH2:9]2)=[CH:4][C:3]=1[O:19][CH3:20].CC(C[AlH]CC(C)C)C>C1COCC1.C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[CH2:9][CH2:10][C:11](=[CH:14][CH2:15][OH:16])[CH2:12][CH2:13]2)=[CH:4][C:3]=1[O:19][CH3:20]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14487Diisobutylaluminum hydrideHCID 68557054HCID 68557054、化合物

生成物 1

HCID 685548602-(1-(4-Chloro-3-methoxyphenyl)piperidin-4-ylidene)ethanol収率 102%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

A solution of methyl 2-(1-(4-chloro-3-methoxyphenyl)piperidin-4-ylidene)acetate (275 mg, 0.930 mmol) in anhydrous THF (3 mL) was cooled to −78° C. and then treated with DIBAL-H (3.72 mL of a 1.0 M solution in toluene, 3.72 mmol). The reaction was stirred at −78° C. for 2.5 h and then quenched with EtOAc. After it warmed to 0° C., the mixture was treated with saturated potassium sodium tartrate solution and stirred vigorously for 20 min. The resulting mixture was extracted with EtOAc. The extract was dried (Na2SO4) and concentrated to give a yellow oil, which was purified by flash chromatography (4 g silica gel cartridge and gradient elution with EtOAc/hexanes) to give 2-(1-(4-chloro-3-methoxyphenyl)piperidin-4-ylidene)ethanol (253 mg, 0.945 mmol, 102% yield) as a yellow oil. 1H-NMR (400 MHz, CDCl3) δ ppm 7.18 (1 H, d, J=8.79 Hz), 6.48 (1 H, d, J=16.92 Hz), 6.43 (1 H, s), 5.50 (1 H, t, J=7.03 Hz), 4.18 (2 H, d, J=7.03 Hz), 3.87 (3 H, s), 3.22 (4 H, dt, J=9.50, 5.68 Hz), 2.39-2.48 (2 H, m), 2.32-2.39 (2 H, m).

後処理

  1. customquenched with EtOAc
  2. temperatureAfter it warmed to 0° C.
  3. additionthe mixture was treated with saturated potassium sodium tartrate solution
  4. stirringstirred vigorously for 20 min
  5. extractionThe resulting mixture was extracted with EtOAc
  6. dry with materialThe extract was dried (Na2SO4)
  7. concentrationconcentrated
  8. customto give a yellow oil, which
  9. customwas purified by flash chromatography (4 g silica gel cartridge and gradient elution with EtOAc/hexanes)

出典と根拠

ORDレコード
ord-c34a7cb1d6d347198f40a03e9ec38025
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08354432B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート