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

HRID 1716528ノート

反応式

HRID 1716528 の反応式
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]

参加物

6

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-26fc5a5b0a19465595cbb08041ca5aa1
出典データセット
uspto-grants-2010_09
特許番号
US07803801B2

反応ノート

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