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

Hydrochloric Acid → 7-Hydroxy-3-(4-hydroxyphenyl)-3-methyl-4-(2-propenyl)chroman

HRID 1267495
ノート
印刷プレビュー

反応式

HRID 1267495 の反応式
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6](=O)[C:7]([C:13]3[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=3)([CH3:12])[CH2:8][O:9]2)=[CH:4][CH:3]=1.[H-].[CH2:22]([Al+]CC(C)C)[CH:23](C)[CH3:24].C1(C)C=CC=CC=1.[Cl-].[NH4+].Cl.C([Si](C)(C)C)C=C>O1CCCC1.ClCCCl.[I-].[Zn+2].[I-].CO>[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]([CH2:24][CH:23]=[CH2:22])[C:7]([C:13]3[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=3)([CH3:12])[CH2:8][O:9]2)=[CH:4][CH:3]=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

11

反応物 6

HCID 313Hydrochloric Acid2 回HCID 1140TolueneHCID 25517Ammonium Chloride2 回HCID 69808AllyltrimethylsilaneHCID 21225700DiisobutylaluminumhydrideHCID 22033150HCID 22033150、化合物

生成物 1

HCID 23001693
7-Hydroxy-3-(4-hydroxyphenyl)-3-methyl-4-(2-propenyl)chroman
収率 44%

試薬・触媒・溶媒 4

HCID 9883512zinc(II)iodide触媒HCID 111,2-Dichloroethane溶媒HCID 887Methanol溶媒2 回HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-78 °C

実験手順

The (+)-7-hydroxy-3-(4-hydroxyphenyl)-3-methylchroman-4-one resolved as Peak 1 in Example 22 (2.0 g, 7.40 mmol) was dissolved in anhydrous tetrahydrofuran (30 ml) and then cooled to −78° C. To this solution, a solution of diisobutylaluminum hydride in toluene (1N, 22.94 ml, 22.94 mmol) was slowly added dropwise, and the resulting mixture was stirred for 35 minutes at −78° C. Methanol (1 ml) was added to the reaction mixture at −78° C., which was then warmed to 0° C. and saturated aqueous ammonium chloride (5 ml) and concentrated hydrochloric acid (7 ml) were added to the mixture followed by stirring for 30 minutes. The reaction mixture was extracted twice with ethyl acetate. The combined organic layers were washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. After distilling off the solvent, zinc iodide (2.55 g, 7.98 mmol) was added to a suspension of the residue and allyltrimethylsilane (5.3 ml, 33.2 mmol) in 1,2-dichloroethane (80 ml) followed by stirring for 12 hours at room temperature. Saturated aqueous ammonium chloride (15 ml), methanol (10 ml) and concentrated hydrochloric acid (10 ml) were added to the reaction mixture, followed by stirring for 30 minutes. The reaction mixture was extracted twice with dichloromethane. The combined organic layers were washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. After distilling off the solvent, the residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/4) to give optically active 7-hydroxy-3-(4-hydroxyphenyl)-3-methyl-4-(2-propenyl)chroman (cis-configuration, 859 mg, Yield 44%).

後処理

  1. temperaturewhich was then warmed to 0° C.
  2. stirringby stirring for 30 minutes
  3. extractionThe reaction mixture was extracted twice with ethyl acetate
  4. washThe combined organic layers were washed with water and saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. stirringby stirring for 12 hours at room temperature
  7. stirringby stirring for 30 minutes
  8. extractionThe reaction mixture was extracted twice with dichloromethane
  9. washThe combined organic layers were washed with water and saturated aqueous sodium chloride
  10. dry with materialdried over anhydrous magnesium sulfate
  11. distillationAfter distilling off the solvent
  12. customthe residue was purified by silica gel column chromatography (eluent: ethyl acetate/hexane=1/4)

出典と根拠

ORDレコード
ord-05429bc7aa75493b971a3faaa7f4f3cb
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06552069B1

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