Water → alpha-[[(Acetyloxy)methoxy]carbonyl]-(2,3-dihydro-5-benzofuranyl)acetic acid

HRID 1390226노트

반응식

HRID 1390226 반응식
[C:1]([CH:4]([C:8]1[CH:9]=[CH:10][C:11]2[O:15][CH2:14][CH2:13][C:12]=2[CH:16]=1)[C:5]([OH:7])=[O:6])([OH:3])=[O:2].O.Cl[CH2:19][O:20][C:21](=[O:23])[CH3:22].C(OCC)(=O)C>[OH-].[Na+].CCOCC>[C:21]([O:20][CH2:19][O:6][C:5]([CH:4]([C:8]1[CH:9]=[CH:10][C:11]2[O:15][CH2:14][CH2:13][C:12]=2[CH:16]=1)[C:1]([OH:3])=[O:2])=[O:7])(=[O:23])[CH3:22]

참가 물질

7

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 69366Chloromethyl acetateHCID 23335822alpha-Carboxy(2,3-dihydro-5-benzofuranyl)acetic acid

생성물 1

HCID 22748513alpha-[[(Acetyloxy)methoxy]carbonyl]-(2,3-dihydro-5-benzofuranyl)acetic acid

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 14798Sodium Hydroxide용매

실험 절차

α-Carboxy(2,3-dihydro-5-benzofuranyl)acetic acid (10 mmole) is dissolved in 50 ml of water containing 10 mmole of sodium hydroxide. This mixture is stirred for 30 minutes at room temperature and then 10 mmole of chloromethylacetate in 25 ml of ether is added. The temperature during the addition is 10° C.; after the addition is complete, the temperature is raised to 20° C. and the mixture stirred for an additional 30 minutes. The pH is adjusted to 2 and ethyl acetate is added. The organic phase is removed, dried over magnesium sulfate, filtered and evaporated to give the title compound.

후처리

  1. additionThe temperature during the addition
  2. customis 10° C.
  3. additionafter the addition
  4. temperaturethe temperature is raised to 20° C.
  5. stirringthe mixture stirred for an additional 30 minutes
  6. additionis added
  7. customThe organic phase is removed
  8. dry with materialdried over magnesium sulfate
  9. filtrationfiltered
  10. customevaporated

출처 및 근거

ORD 기록
ord-9e27995e46394986b44adfacae2803fa
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04138397

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