Sodium Hydroxide → [3-{1-[(Benzoyloxy)carbonyl]piperidin-4-yl}-2-oxotetrahydropyrimidin-1(2H)-yl]acetic acid

HRID 2366546

反応式

HRID 2366546 の反応式
[OH-:1].[Na+].C([O:7][C:8]([CH2:10][N:11]1[CH2:16][CH2:15][CH2:14][N:13]([CH:17]2[CH2:22][CH2:21][N:20]([C:23]([O:25][CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[O:24])[CH2:19][CH2:18]2)[C:12]1=[O:33])=[O:9])(C)(C)C>C(O)C>[C:26]([O:25][C:23]([N:20]1[CH2:21][CH2:22][CH:17]([N:13]2[CH2:14][CH2:15][CH2:16][N:11]([CH2:10][C:8]([OH:7])=[O:9])[C:12]2=[O:33])[CH2:18][CH2:19]1)=[O:24])(=[O:1])[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 68417510benzyl 4-[3-(tert-butoxycarbonylmethyl)-2-oxotetrahydropyrimidin-1(2H)-yl]piperidin-1-carboxylate

生成物 1

HCID 86623802[3-{1-[(Benzoyloxy)carbonyl]piperidin-4-yl}-2-oxotetrahydropyrimidin-1(2H)-yl]acetic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

An aqueous 4N sodium hydroxide solution (10 mL) was added to a solution of benzyl 4-[3-(tert-butoxycarbonylmethyl)-2-oxotetrahydropyrimidin-1(2H)-yl]piperidin-1-carboxylate (1.7 g) obtained in Example 35a) in ethanol (20 mL), and the mixture was stirred at room temperature overnight. Ethanol was distilled off under reduced pressure, and 1N hydrochloric acid was added to the residue to adjust pH to 3, followed by extraction with chloroform. The extract was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain the title compound (1.5 g, quantitative) as a white powder.

後処理

  1. distillationEthanol was distilled off under reduced pressure, and 1N hydrochloric acid
  2. additionwas added to the residue
  3. extractionfollowed by extraction with chloroform
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f0f2673aed344381a9eeb7d5c2dac239
出典データセット
uspto-grants-2014_04
特許番号
US08697865B2

関連ノート

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