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

Trifluoroacetic acid → 3-(2,4-Dihydroxy-phenyl)-7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one

HRID 61867
ノート
印刷プレビュー

反応式

HRID 61867 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][C:9](=[O:15])[C:10]2([CH3:14])[CH3:13])=[CH:5][CH:4]=1.C[C:17]([CH3:20])([O-:19])[CH3:18].[Na+].F[B-](F)(F)F.[C:27]([PH+](C(C)(C)C)C(C)(C)C)([CH3:30])(C)[CH3:28].FC(F)(F)C(O)=[O:43].P([O-])([O-])(O)=O.[K+].[K+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(Cl)Cl.CO.C1(C)C=CC=CC=1>[OH:43][C:28]1[CH:20]=[C:17]([OH:19])[CH:18]=[CH:30][C:27]=1[CH:8]1[CH2:7][C:6]2[C:11](=[CH:12][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[C:10]([CH3:13])([CH3:14])[C:9]1=[O:15]
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

10

反応物 5

HCID 6422Trifluoroacetic acidHCID 24450Potassium Phosphate, DibasicHCID 2734635Tri-tert-butylphosphine tetrafluoroborateHCID 130110077-Methoxy-1,1-dimethyl-3,4-dihydronaphthalen-2(1H)-one2 回HCID 23676156Sodium t-butoxide

生成物 1

HCID 66834619
3-(2,4-Dihydroxy-phenyl)-7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one
収率 36%

試薬・触媒・溶媒 4

HCID 167845palladium(II) acetate触媒HCID 887Methanol溶媒HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
70 °C

実験手順

To 7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound A2, 10 g), 2-bromo-1,3-dihydroxytetrahydropyranbenzene (Compound Z9, 20.98 g), sodium t-butoxide (5.88 g), palladium acetate (550 mg) and tri-t-butylphosphonium tetrafluoroborate (710 mg), toluene (40 mL) was added and the mixture was stirred and heated at 70° C. under nitrogen atmosphere for 6 hr. After cooling, the reaction mixture was added with methanol (38 mL) and trifluoroacetic acid (14.54 mL) at room temperature, and then stirred at room temperature overnight. To the resulting residues, methylene chloride and saturated dipotassium hydrogen phosphate were added and the organic layer was washed with saturated brine. Thereafter, the organic layer was dried over magnesium sulfate. The residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound (5.53 g, 36%).

後処理

  1. temperatureAfter cooling
  2. stirringstirred at room temperature overnight
  3. washthe organic layer was washed with saturated brine
  4. dry with materialThereafter, the organic layer was dried over magnesium sulfate
  5. customThe residues obtained
  6. concentrationafter concentration under reduced pressure
  7. customwere purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-0efc1906e96e4b0f843e4ee769e03666
出典データセット
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09440922B2

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