Tetrahydrofuran → 3-Ethoxy-3-oxo-2-{4-[2-(2-oxo-1,3-benzoxazol-3(2H)-yl)ethoxy]benzyl}propanoic acid

HRID 896484노트

반응식

HRID 896484 반응식
[O:1]=[C:2]1[N:6]([CH2:7][CH2:8][O:9][C:10]2[CH:27]=[CH:26][C:13]([CH2:14][CH:15]([C:21]([O:23]CC)=[O:22])[C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:12][CH:11]=2)[C:5]2[CH:28]=[CH:29][CH:30]=[CH:31][C:4]=2[O:3]1.O1CCCC1.[OH-].[Na+]>C(O)C>[CH2:19]([O:18][C:16](=[O:17])[CH:15]([CH2:14][C:13]1[CH:12]=[CH:11][C:10]([O:9][CH2:8][CH2:7][N:6]2[C:5]3[CH:28]=[CH:29][CH:30]=[CH:31][C:4]=3[O:3][C:2]2=[O:1])=[CH:27][CH:26]=1)[C:21]([OH:23])=[O:22])[CH3:20]

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 10159558Diethyl 2-{4-[2-(2-oxo-1,3-benzoxazol-3(2H)-yl)ethoxy]benzyl}malonate

생성물 1

HCID 101790283-Ethoxy-3-oxo-2-{4-[2-(2-oxo-1,3-benzoxazol-3(2H)-yl)ethoxy]benzyl}propanoic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Dissolve the compound obtained in Example 2 (0.5 g) in absolute ethanol (6.5 ml) and add tetrahydrofuran (2 ml). Subsequently, cool the reaction mixture using an ice bath and add 2N sodium hydroxide (0.7 ml). Stir magnetically for 18 hours at ambient temperature. Remove the absolute ethanol/tetrahydrofuran mixture by evaporation under reduced pressure. Take up the resulting residue in water and extract twice with 50 ml of ether each time. Acidify the aqueous phase with a 6N hydrochloric acid solution until a pH of 1 is obtained, then extract twice with 50 ml of ether each time. Dry the organic phase over magnesium sulphate and remove the ether by evaporation under reduced pressure.

후처리

  1. temperatureSubsequently, cool the reaction mixture
  2. customRemove the absolute ethanol/tetrahydrofuran mixture
  3. customby evaporation under reduced pressure
  4. extractionextract twice with 50 ml of ether each time
  5. customis obtained
  6. extractionextract twice with 50 ml of ether each time
  7. dry with materialDry the organic phase over magnesium sulphate
  8. customremove the ether
  9. customby evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-46d3b8e4999f48e5a8504d0dd0554259
출처 데이터셋
uspto-grants-2005_07
특허 번호
US06919362B2

반응 노트

불러오는 중…