1,2-Dibromoethane → Methyl 2,3-dihydro-1,4-benzodioxine-6-carboxylate

HRID 596602노트

반응식

HRID 596602 반응식
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([OH:11])[CH:5]=1.C[O-].[Na+].Br[CH2:17][CH2:18]Br>CO>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]2[O:10][CH2:17][CH2:18][O:11][C:6]=2[CH:5]=1

참가 물질

5

반응물 3

HCID 78391,2-DibromoethaneHCID 287064Methyl 3,4-DihydroxybenzoateHCID 10942334Sodium Methoxide

생성물 1

HCID 3802178Methyl 2,3-dihydro-1,4-benzodioxine-6-carboxylate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 4.20 g. of 3,4-dihydroxybenzoic acid methyl ester in 10.0 ml. of methanol is combined with 7.0 g. of sodium methoxide and then 15.0 g. of 1,2-dibromoethane is added. The resulting mixture is refluxed under nitrogen for 24 hours, then cooled, filtered, evaporated in vacuo and the resulting oil dissolved in 50 ml. of chloroform. The resulting solution after again filtering is chromatographed over 100 ml. of silica gel eluting with chloroform to obtain 3,4-ethylenedioxybenzoic acid methyl ester, m.p. 43°-45° C.

후처리

  1. temperatureThe resulting mixture is refluxed under nitrogen for 24 hours
  2. temperaturecooled
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. dissolutionthe resulting oil dissolved in 50 ml
  6. filtrationThe resulting solution after again filtering
  7. customis chromatographed over 100 ml

출처 및 근거

ORD 기록
ord-a68d6c679ea04501b26a9aae8c2ed78d
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04011323

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