Lithium hydroxide, monohydrate → 3-{4-[2-(4-tert-Butoxycarbonylaminophenyl)ethoxy]phenyl}-2-ethoxypropanoic acid

HRID 987149노트

반응식

HRID 987149 반응식
O.[OH-].[Li+].[C:4]([O:8][C:9]([NH:11][C:12]1[CH:17]=[CH:16][C:15]([CH2:18][CH2:19][O:20][C:21]2[CH:26]=[CH:25][C:24]([CH2:27][CH:28]([O:34][CH2:35][CH3:36])[C:29]([O:31]CC)=[O:30])=[CH:23][CH:22]=2)=[CH:14][CH:13]=1)=[O:10])([CH3:7])([CH3:6])[CH3:5]>O.C1COCC1>[C:4]([O:8][C:9]([NH:11][C:12]1[CH:13]=[CH:14][C:15]([CH2:18][CH2:19][O:20][C:21]2[CH:22]=[CH:23][C:24]([CH2:27][CH:28]([O:34][CH2:35][CH3:36])[C:29]([OH:31])=[O:30])=[CH:25][CH:26]=2)=[CH:16][CH:17]=1)=[O:10])([CH3:7])([CH3:6])[CH3:5]

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 22988408Ethyl 3-(4-[2-(4-tert-butoxycarbonylaminophenyl)ethoxy]phenyl}-2-ethoxypropanoate

생성물 1

HCID 229884463-{4-[2-(4-tert-Butoxycarbonylaminophenyl)ethoxy]phenyl}-2-ethoxypropanoic acid수율 98.7%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Lithium hydroxide hydrate (77 mg; 1.85 mmole) in water (5.5 ml) was slowly added to a solution of ethyl 3-{4-[2-(4-tert-butoxycarbonylaminophenyl)ethoxy]phenyl}-2-ethoxypropanoate (0.77 g; 1.68 mmole) in THF (7.6 ml). After stirring at room temperature for 4 hours the reaction mixture was kept in a freezer for 4 days. THP was removed by evaporation in vacuo. More water was added and the mixture was acidified with hydrochloric acid to pH1. The product was extracted with ethyl acetate, washed twice with water, dried (sodium sulfate), filtered and the solvent was evaporated in vacuo to give 0.712 g (98.7% yield) of the desired product.

후처리

  1. waitwas kept in a freezer for 4 days
  2. customTHP was removed by evaporation in vacuo
  3. additionMore water was added
  4. extractionThe product was extracted with ethyl acetate
  5. washwashed twice with water
  6. dry with materialdried (sodium sulfate)
  7. filtrationfiltered
  8. customthe solvent was evaporated in vacuo

출처 및 근거

ORD 기록
ord-7fe98255f20848428378b07fd7d97b78
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06630509B2

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