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

HRID 2366546

반응식

HRID 2366546 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f0f2673aed344381a9eeb7d5c2dac239
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08697865B2

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