Water → Maltol

HRID 1164270

반응식

HRID 1164270 반응식
[OH2:1].[Br-].[Na+].[O:4]1[CH:8]=[CH:7][CH:6]=[C:5]1[CH:9]([OH:11])[CH3:10].ClCl>O1CCCC1>[CH3:10][C:9]1[O:11][CH:8]=[CH:7][C:6](=[O:1])[C:5]=1[OH:4]

참가 물질

6

반응물 4

HCID 962WaterHCID 24526Chlorine2회HCID 1072431-(2-Furyl)ethanolHCID 253881Sodium Bromide

생성물 1

HCID 8369Maltol수율 55%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
10 °C

실험 절차

In a 3-neck round bottom flask equipped with a stirring bar, a gas inlet tube and an addition funnel was added 20 ml of tetrahydrofuran, 50 ml of water and sodium bromide (0.20 mole). The solution was cooled to a temperature of 0 to 20° C. The addition funnel was charged with a solution of 1(2-furyl)-1-ethanol (0.18 mole) in 20 ml of tetrahydrofuran and this was added dropwise to the rapidly stirred reaction flask while gaseous chlorine (0.40 mole) is added via the gaseous inlet tube. The rate of the alcohol addition was such that a yellow orange color was maintained. The reaction temperature was kept below 20° C. with ice bath cooling. After the alcohol and chlorine had both been added to the reaction flask, the temperature was raised to reflux to distill off the tetrahydrofuran. The isolation procedure of Example 1 was used to isolate 12.47 g of pure maltol (55% yield).

후처리

  1. customIn a 3-neck round bottom flask equipped with a stirring bar, a gas inlet tube and an addition funnel
  2. additionis added via the gaseous inlet tube
  3. temperaturewas maintained
  4. customThe reaction temperature was kept below 20° C. with ice bath
  5. temperaturecooling
  6. additionboth been added to the reaction flask
  7. temperaturethe temperature was raised
  8. temperatureto reflux
  9. distillationto distill off the tetrahydrofuran

출처 및 근거

ORD 기록
ord-8b0ab203ba2540f9bc4fe8a0e4daf1f7
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04368331

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