Water → HCID 178524913, 화합물

HRID 2169201노트

반응식

HRID 2169201 반응식
C([O:5][C:6]([C:8]1[NH:9][C:10]([CH2:23][C:24]2[C:29]([Cl:30])=[CH:28][CH:27]=[CH:26][C:25]=2[Cl:31])=[N:11][C:12](=[O:22])[C:13]=1[O:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:7])(C)(C)C.[Li+].[OH-].O>O1CCCC1>[CH2:15]([O:14][C:13]1[C:12](=[O:22])[N:11]=[C:10]([CH2:23][C:24]2[C:25]([Cl:31])=[CH:26][CH:27]=[CH:28][C:29]=2[Cl:30])[NH:9][C:8]=1[C:6]([OH:7])=[O:5])[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 178450869HCID 178450869, 화합물

생성물 1

HCID 178524913HCID 178524913, 화합물수율 95.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

5-(Benzyloxy)-2-(2,6-dichlorobenzyl)-6-oxo-3,6-dihydro-pyrimidine-4-carboxylic acid tert-butyl ester (61) (0.24 g, 520 μmol, Eq: 1.00) and LiOH (62.3 mg, 2.6 mmol, Eq: 5) were stirred in tetrahydrofuran (2 ml)/water (1.00 ml) at reflux overnight. The solvent was mostly removed. The residue was taken up in water and was extracted once with ethyl acetate. The aqueous layer was acidified with HCl conc. The precipitate was collected by filtration, washed with water and dried to afford 5-benzyloxy-2-(2,6-dichlorobenzyl)-6-oxo-3,6-dihydro-pyrimidine-4-carboxylic acid (62) (0.202 g, 498 μmol, 95.8% yield) as a white solid.

후처리

  1. temperatureat reflux overnight
  2. customThe solvent was mostly removed
  3. extractionwas extracted once with ethyl acetate
  4. filtrationwas collected by filtration
  5. washwashed with water
  6. customdried

출처 및 근거

ORD 기록
ord-0bd0c22926f340129ad0a84f9c4a70ef
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09045486B2

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