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

HRID 1175194
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HRID 1175194 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

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.

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후처리

  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

출처 및 근거

ORD 기록
ord-bff1d313d43f4143960cbb83b4029bc5
출처 데이터셋
uspto-grants-2010_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07838688B2

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