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

Sodium Carbonate → 6-tert-Butyl-4-(3,5-di-tert-butylphenyl)-5-methoxy-2-methylindan-1-one

HRID 716468
ノート
印刷プレビュー

反応式

HRID 716468 の反応式
Br[C:2]1[C:10]([O:11][CH3:12])=[C:9]([C:13]([CH3:16])([CH3:15])[CH3:14])[CH:8]=[C:7]2[C:3]=1[CH2:4][CH:5]([CH3:18])[C:6]2=[O:17].[C:19]([C:23]1[CH:24]=[C:25](B(O)O)[CH:26]=[C:27]([C:29]([CH3:32])([CH3:31])[CH3:30])[CH:28]=1)([CH3:22])([CH3:21])[CH3:20].C([O-])([O-])=O.[Na+].[Na+].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>CC([O-])=O.CC([O-])=O.[Pd+2].COCCOC.O>[C:13]([C:9]1[CH:8]=[C:7]2[C:3]([CH2:4][CH:5]([CH3:18])[C:6]2=[O:17])=[C:2]([C:25]2[CH:24]=[C:23]([C:19]([CH3:21])([CH3:20])[CH3:22])[CH:28]=[C:27]([C:29]([CH3:32])([CH3:31])[CH3:30])[CH:26]=2)[C:10]=1[O:11][CH3:12])([CH3:16])([CH3:15])[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 11470330(3,5-Di-tert-butylphenyl)boronic acidHCID 602106934-Bromo-6-tert-butyl-5-methoxy-2-methyl-1-indanone

生成物 1

HCID 712309426-tert-Butyl-4-(3,5-di-tert-butylphenyl)-5-methoxy-2-methylindan-1-one収率 44.6%

試薬・触媒・溶媒 3

HCID 167845
palladium(II) acetate
触媒
HCID 962Water溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

A mixture of 30.7 g (98.6 mmol) of 4-bromo-6-tertbutyl-5-methoxy-2-methylindanone, 30.6 g (128 mmol) 3,5-di-tert-butylphenylboronic acid, 29.7 g (280 mmol) of Na2CO3, 1.35 g (5.92 mmol; 6 mol. %) of Pd(OAc)2, 3.15 g (11.8 mmol; 12 mol. %) of PPh3, 130 ml of water, and 380 ml of 1,2-dimethoxyethane was refluxed for 12 h. Further on, the reaction mixture was quenched with water, solvents were evaporated. The residue was dissolved in 500 ml of dichloromethane, and this solution was washed by 500 ml of water. The organic layer was separated, the aqueous layer was additionally extracted with 100 ml of dichloromethane. The combined organic extract was dried over Na2SO4, then evaporated to dryness. The crude product isolated from the residue using flash chromatography on silica gel 60 (40-63 um, hexanes-dichloromethane=2:1, vol.) was then re-crystallized from n-hexane to give 18.5 g (43%) of a white solid.

後処理

  1. temperaturewas refluxed for 12 h
  2. customFurther on, the reaction mixture was quenched with water, solvents
  3. customwere evaporated
  4. dissolutionThe residue was dissolved in 500 ml of dichloromethane
  5. washthis solution was washed by 500 ml of water
  6. customThe organic layer was separated
  7. extractionthe aqueous layer was additionally extracted with 100 ml of dichloromethane
  8. extractionThe combined organic extract
  9. dry with materialwas dried over Na2SO4
  10. customevaporated to dryness
  11. customThe crude product isolated from the residue
  12. customwas then re-crystallized from n-hexane

出典と根拠

ORDレコード
ord-b9e4156dc0cc46088184d8b37d8eff08
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09187583B2

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