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Potassium Acetate → (2,3-Dihydrothieno[3,4-b]-1,4-dioxin-2-yl)methyl acetate

HRID 1175194
ノート
印刷プレビュー

反応式

HRID 1175194 の反応式
Br[CH2:2][CH:3]1[O:8][C:7]2=[CH:9][S:10][CH:11]=[C:6]2[O:5][CH2:4]1.[C:12]([O-:15])(=[O:14])[CH3:13].[K+]>CS(C)=O>[C:12]([O:15][CH2:2][CH:3]1[O:8][C:7]2=[CH:9][S:10][CH:11]=[C:6]2[O:5][CH2:4]1)(=[O:14])[CH3:13]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 517044Potassium AcetateHCID 569236862-(Bromomethyl)-2,3-dihydrothieno[3,4-b][1,4]dioxine

生成物 1

HCID 59558874(2,3-Dihydrothieno[3,4-b]-1,4-dioxin-2-yl)methyl acetate収率 90%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

In a 50 mL Schlenk tube 1.00 g of to 2-(bromomethyl)-2,3-dihydrothieno[3,4-b][1,4]dioxine was combined with 0.5 g (0.0051 mol) potassium acetate and 25 mL DMSO. The tube was sealed and stirred for 1 h at 100 C. At this time TLC indicated complete consumption of starting material. The reaction was poured into water and extracted with ether. After removing the ether under reduced pressure column chromatography was performed using 90% methylene chloride in hexane to isolate a light yellow oil in 90% yield. The structure and purity were confirmed by 1H/13C NMR and GC-MS.

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

後処理

  1. customThe tube was sealed
  2. customconsumption of starting material
  3. additionThe reaction was poured into water
  4. extractionextracted with ether
  5. customAfter removing the ether under reduced pressure column chromatography
  6. customto isolate a light yellow oil in 90% yield

出典と根拠

ORDレコード
ord-bff1d313d43f4143960cbb83b4029bc5
出典データセット
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07838688B2

反応ノート

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