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

Ethyl phenylacetate → Ethyl 3-(2,3-dihydrobenzofuran-5-yl)-2-phenylpropionate

HRID 1636608
ノート
印刷プレビュー

反応式

HRID 1636608 の反応式
C[Si](C)(C)[N-][Si](C)(C)C.[Li+].C[Si](C)(C)N[Si](C)(C)C.C([Li])CCC.[C:25]1([CH2:31][C:32]([O:34][CH2:35][CH3:36])=[O:33])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1.Br[CH2:38][C:39]1[CH:40]=[CH:41][C:42]2[O:46][CH2:45][CH2:44][C:43]=2[CH:47]=1>O1CCCC1.O>[O:46]1[C:42]2[CH:41]=[CH:40][C:39]([CH2:38][CH:31]([C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[C:32]([O:34][CH2:35][CH3:36])=[O:33])=[CH:47][C:43]=2[CH2:44][CH2:45]1
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 5

HCID 7590Ethyl phenylacetateHCID 13838HexamethyldisilazaneHCID 2733832Lithium hexamethyldisilazaneHCID 220048075-(Bromomethyl)-2,3-dihydrobenzofuranHCID 178418339Butyllithium

生成物 1

HCID 22004839Ethyl 3-(2,3-dihydrobenzofuran-5-yl)-2-phenylpropionate

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒3 回

実験手順

To a solution of lithium hexamethyldisilazide solution, prepared from 1,1,1,3,3,3-hexamethyldisilazane (37.4 g, 0.232 mol), n-butyllithium (127 mL, 1.6 M hexane solution) and tetrahydrofuran (150 mL), was added a solution of ethyl phenylacetate (33.3 g, 0.203 mol) in tetrahydrofuran (20 mL) at -78° C. The mixture was stirred for 15 minutes and then a solution of 5-bromomethyl-2,3-dihydrobenzofuran (41.0 g, 0.193 mol) in tetrahydrofuran (50 mL) was added. The mixture was stirred for further 20 minutes, diluted with water and warmed up to room temperature. The product was extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to afford the title compound as an oily product (yield 54.5 g, 95%).

後処理

  1. stirringThe mixture was stirred for further 20 minutes
  2. extractionThe product was extracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated
  6. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)

出典と根拠

ORDレコード
ord-e97a7ba2af0b4130921f553cfb28c8f9
出典データセット
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06034239

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