Water → HCID 178524913、化合物

HRID 2169201ノート

反応式

HRID 2169201 の反応式
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

参加物

5

反応物 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 178450869HCID 178450869、化合物

生成物 1

HCID 178524913HCID 178524913、化合物収率 95.8%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0bd0c22926f340129ad0a84f9c4a70ef
出典データセット
uspto-grants-2015_06
特許番号
US09045486B2

反応ノート

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