Hydrochloric Acid → 2-Methyl-2-(1-{5-[6-(4-methylpyridin-2-ylamino)pyridin-2-yl]thiazol-2-yl}piperidin-4-yl)propionic acid

HRID 1716528노트

반응식

HRID 1716528 반응식
C([O:3][C:4](=[O:33])[C:5]([CH3:32])([CH:7]1[CH2:12][CH2:11][N:10]([C:13]2[S:14][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([NH:24][C:25]4[CH:30]=[C:29]([CH3:31])[CH:28]=[CH:27][N:26]=4)[N:19]=3)=[CH:16][N:17]=2)[CH2:9][CH2:8]1)[CH3:6])C.[OH-].[Na+].Cl>CO.O1CCCC1>[CH3:32][C:5]([CH:7]1[CH2:12][CH2:11][N:10]([C:13]2[S:14][C:15]([C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([NH:24][C:25]4[CH:30]=[C:29]([CH3:31])[CH:28]=[CH:27][N:26]=4)[N:19]=3)=[CH:16][N:17]=2)[CH2:9][CH2:8]1)([CH3:6])[C:4]([OH:33])=[O:3]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 587067352-Methyl-2-(1-{5-[6-(4-methylpyridin-2-ylamino)pyridin-2-yl]thiazol-2-yl}piperidin-4-yl)propionic acid ethyl ester

생성물 1

HCID 441766832-Methyl-2-(1-{5-[6-(4-methylpyridin-2-ylamino)pyridin-2-yl]thiazol-2-yl}piperidin-4-yl)propionic acid수율 67%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a mixed solution of 2-methyl-2-(1-{5-[6-(4-methylpyridin-2-ylamino)pyridin-2-yl]thiazol-2-yl}piperidin-4-yl)propionic acid ethyl ester (697 mg, 1.50 mmol) obtained in Step 3 in methanol (5 ml) and tetrahydrofuran (10 ml), 4N aqueous sodium hydroxide (3.7 ml, 15 mmol) was added and the mixture was stirred for 15 hours under refluxing. After concentrated, the reaction solution was neutralized with 1N hydrochloric acid (15 ml, 15 mmol), and the precipitated solid was collected by filtration, washed with water, ethyl acetate, tetrahydrofuran. After dried in vacuo, the title compound (438 mg, 67%) was obtained.

후처리

  1. temperatureunder refluxing
  2. concentrationAfter concentrated
  3. filtrationthe precipitated solid was collected by filtration
  4. washwashed with water, ethyl acetate, tetrahydrofuran
  5. customAfter dried in vacuo

출처 및 근거

ORD 기록
ord-26fc5a5b0a19465595cbb08041ca5aa1
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803801B2

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