Hydrochloric Acid → HCID 14126617, 화합물

HRID 703655

반응식

HRID 703655 반응식
[C:1]1(=[O:17])[N:5]([CH2:6][CH2:7][O:8][CH2:9][CH2:10][OH:11])[C:4](=[O:12])[C:3]2=[CH:13][CH:14]=[CH:15][CH:16]=[C:2]12.[H-].[Na+].Cl[CH2:21][C:22](=[O:29])[CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25].Cl>O1CCCC1>[CH2:27]([O:26][C:24](=[O:25])[CH2:23][C:22](=[O:29])[CH2:21][O:11][CH2:10][CH2:9][O:8][CH2:7][CH2:6][N:5]1[C:4](=[O:12])[C:3]2=[CH:13][CH:14]=[CH:15][CH:16]=[C:2]2[C:1]1=[O:17])[CH3:28]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 24758Sodium hydrideHCID 69484Ethyl 4-chloroacetoacetateHCID 27554062-(2-(2-Hydroxyethoxy)ethyl)-1H-isoindole-1,3(2H)-dione

생성물 1

HCID 14126617HCID 14126617, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
25 °C

실험 절차

77 g of 2-[2-(phthalimido)ethoxy]ethanol are added, in portions, to a suspension of 31 g of sodium hydride in 400 ml of tetrahydrofuran, while maintaining the temperature in the vicinity of 25° C. The mixture is stirred for one hour and 53.6 g of ethyl chloroacetoacetate are then added, while maintaining the temperature of the mixture at -20° C. The mixture is allowed to stand overnight at ambient temperature and then hydrolyzed with 1 l of 1N hydrochloric acid. Decantation, followed by extraction with ether are carried out and the organic phases are combined. The combined organic phase is washed with water and then dried over magnesium sulfate. It is concentrated and the residue thereby obtained (110 g) is purified by silica column chromatography using a dichloromethane:acetone (95:5) mixture as the eluting solvent. After removing the eluting solvent, 35.7 g of 10-phthalimido-3-oxo-5,8-dioxadecanoic acid ethyl ester are obtained.

후처리

  1. temperaturewhile maintaining the temperature of the mixture at -20° C
  2. waitto stand overnight at ambient temperature
  3. extractionDecantation, followed by extraction with ether
  4. washThe combined organic phase is washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationIt is concentrated
  7. customthe residue thereby obtained (110 g)
  8. customis purified by silica column chromatography
  9. customAfter removing the eluting solvent, 35.7 g of 10-phthalimido-3-oxo-5,8-dioxadecanoic acid ethyl ester
  10. customare obtained

출처 및 근거

ORD 기록
ord-245dfa84df4e493ca754d84d4cd1006a
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04983740

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