Hydrochloric Acid → Acetic acid, (4-(2-(1,3-diethyl-2,3,6,7-tetrahydro-7-methyl-2,6-dioxo-1H-purin-8-yl)ethenyl)phenoxy)-, (E)-

HRID 1077539노트

반응식

HRID 1077539 반응식
C([O:3][C:4]([CH2:6][O:7][C:8]1[CH:31]=[CH:30][C:11](/[CH:12]=[CH:13]/[C:14]2[N:22]([CH3:23])[C:21]3[C:20](=[O:24])[N:19]([CH2:25][CH3:26])[C:18](=[O:27])[N:17]([CH2:28][CH3:29])[C:16]=3[N:15]=2)=[CH:10][CH:9]=1)=[O:5])C.O.[OH-].[Li+].Cl>O1CCCC1.C(O)C.O>[C:4]([CH2:6][O:7][C:8]1[CH:31]=[CH:30][C:11](/[CH:12]=[CH:13]/[C:14]2[N:22]([CH3:23])[C:21]3[C:20](=[O:24])[N:19]([CH2:25][CH3:26])[C:18](=[O:27])[N:17]([CH2:28][CH3:29])[C:16]=3[N:15]=2)=[CH:10][CH:9]=1)([OH:5])=[O:3]

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 6448954Acetic acid, (4-(2-(1,3-diethyl-2,3,6,7-tetrahydro-7-methyl-2,6-dioxo- 1H-purin-8-yl)ethenyl)phenoxy)-, ethyl ester, (E)-

생성물 1

HCID 6448955Acetic acid, (4-(2-(1,3-diethyl-2,3,6,7-tetrahydro-7-methyl-2,6-dioxo-1H-purin-8-yl)ethenyl)phenoxy)-, (E)-수율 21.4%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Compound 189 (200 mg, 0.47 mmol) obtained in Reference Example 186 was dissolved in a mixed solvent of 4 ml of tetrahydrofuran, 4 ml of ethanol, and 2 ml of water. To the solution was added 98 mg (2.34 mmol) of lithium hydroxide monohydrate, and the mixture was stirred at room temperature for one hour. To the reaction solution was added 2N hydrochloric acid, and the mixture was extracted with chloroform and dried over anhydrous sodium sulfate, followed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol/acetic acid) to give 40 mg (yield 21%) of Compound 190 as a pale yellow solid.

후처리

  1. extractionthe mixture was extracted with chloroform
  2. dry with materialdried over anhydrous sodium sulfate
  3. customfollowed by evaporation under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol/acetic acid)

출처 및 근거

ORD 기록
ord-ed23daf32dbb49a9869e24166b283e56
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05543415

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