Lithium Hydroxide → 1-(1-(tert-butoxycarbonyl)piperidin-4-yl)-2-oxo-2,3-dihydro-1H-imidazole-4-carboxylic acid

HRID 1867603노트

반응식

HRID 1867603 반응식
[OH-].[Li+].C[O:4][C:5]([C:7]1[NH:8][C:9](=[O:25])[N:10]([CH:12]2[CH2:17][CH2:16][N:15]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:14][CH2:13]2)[CH:11]=1)=[O:6]>CO>[C:21]([O:20][C:18]([N:15]1[CH2:16][CH2:17][CH:12]([N:10]2[CH:11]=[C:7]([C:5]([OH:6])=[O:4])[NH:8][C:9]2=[O:25])[CH2:13][CH2:14]1)=[O:19])([CH3:24])([CH3:22])[CH3:23]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 68564149HCID 68564149, 화합물

생성물 1

HCID 590063701-(1-(tert-butoxycarbonyl)piperidin-4-yl)-2-oxo-2,3-dihydro-1H-imidazole-4-carboxylic acid수율 35.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Lithium hydroxide (64 mg, 1.54 mmol) was added to a solution of tert-butyl 4-[4-(methoxycarbonyl)-2-oxo-2,3-dihydro-1H-imidazol-1-yl]piperidine-1-carboxylate (50 mg, 0.154 mmol) in methanol (10 mL). After 2 h, the reaction was quenched with saturated sodium bicarbonate solution and dichloromethane was added. The mixture was filtered and the filtrate was concentrated. Purification by silica gel chromatography (100% dichloromethane→25% methanol {1% ammonium hydroxide}/dichloromethane) gave the title compound (17 mg). MS 312.2 (M+1)

후처리

  1. customthe reaction was quenched with saturated sodium bicarbonate solution and dichloromethane
  2. additionwas added
  3. filtrationThe mixture was filtered
  4. concentrationthe filtrate was concentrated
  5. customPurification by silica gel chromatography (100% dichloromethane→25% methanol {1% ammonium hydroxide}/dichloromethane)

출처 및 근거

ORD 기록
ord-97e9ba285e704346b706ff5da4abf22a
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07632832B2

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