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

4-Propylcyclohexanone → 1-(4-Bromo-2-fluorophenyl)-4-propylcyclohexanol

HRID 718492
ノート
印刷プレビュー

反応式

HRID 718492 の反応式
[Li]CCCC.[Br:6][C:7]1[CH:12]=[CH:11][C:10](I)=[C:9]([F:14])[CH:8]=1.[CH2:15]([CH:18]1[CH2:23][CH2:22][C:21](=[O:24])[CH2:20][CH2:19]1)[CH2:16][CH3:17]>C1COCC1>[Br:6][C:7]1[CH:12]=[CH:11][C:10]([C:21]2([OH:24])[CH2:22][CH2:23][CH:18]([CH2:15][CH2:16][CH3:17])[CH2:19][CH2:20]2)=[C:9]([F:14])[CH:8]=1
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 3

HCID 1424824-PropylcyclohexanoneHCID 27245164-Bromo-2-fluoro-1-iodobenzeneHCID 178418339Butyllithium

生成物 1

HCID 680105851-(4-Bromo-2-fluorophenyl)-4-propylcyclohexanol収率 80.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-70 °C

実験手順

Under a nitrogen atmosphere, n-BuLi (108.0 mL, 174.0 mmol) was slowly added dropwise, at −70° C. or lower, to a THF (300 mL) solution of 4-bromo-2-fluoro-1-iodobenzene (67) (50.0 g, 166.0 mmol). The reaction mixture was agitated at −70° C. or lower for 1 hour, and then 4-propylcyclohexanone (66) (24.5 g, 174.0 mmol) was slowly added dropwise thereto. The reaction mixture was returned to room temperature, and then quenched with 200 mL of 1N hydrochloric acid aqueous solution, and extracted with 100 mL of toluene three times. Combined organic layers were washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine, and then dried over magnesium sulfate, and a solvent was distilled off by an evaporator. The residue was purified by silica gel column chromatography, and thus 1-(4-bromo-2-fluorophenyl)-4-propylcyclohexanol (68) (42.0 g, yield 80.2%) was obtained.

後処理

  1. customwas returned to room temperature
  2. customquenched with 200 mL of 1N hydrochloric acid aqueous solution
  3. extractionextracted with 100 mL of toluene three times
  4. washCombined organic layers were washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine
  5. dry with materialdried over magnesium sulfate
  6. distillationa solvent was distilled off by an evaporator
  7. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-0add0333bdc349d8ab777f13d82e21bb
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09193908B2

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