1,4-Dioxane hydrochloride → 2-[(4-{2-[(5-Bromopyridin-2-yl)(heptyl)amino]ethyl}-1,3-thiazol-2-yl)thio]-2-methylpropionic acid hydrochloride

HRID 914426ノート

反応式

HRID 914426 の反応式
C([O:5][C:6](=[O:33])[C:7]([S:10][C:11]1[S:12][CH:13]=[C:14]([CH2:16][CH2:17][N:18]([C:26]2[CH:31]=[CH:30][C:29]([Br:32])=[CH:28][N:27]=2)[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[N:15]=1)([CH3:9])[CH3:8])(C)(C)C.[ClH:34].O1CCOCC1>O1CCOCC1>[ClH:34].[Br:32][C:29]1[CH:30]=[CH:31][C:26]([N:18]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[CH2:17][CH2:16][C:14]2[N:15]=[C:11]([S:10][C:7]([CH3:8])([CH3:9])[C:6]([OH:33])=[O:5])[S:12][CH:13]=2)=[N:27][CH:28]=1

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 597594422-[(4-{2-[(5-Bromopyridin-2-yl)(heptyl)amino]ethyl}-1,3-thiazol-2-yl)thio]-2-methylpropionic acid tert-butyl ester

生成物 1

HCID 673983692-[(4-{2-[(5-Bromopyridin-2-yl)(heptyl)amino]ethyl}-1,3-thiazol-2-yl)thio]-2-methylpropionic acid hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

2-[(4-{2-[(5-Bromopyridin-2-yl)(heptyl)amino]ethyl}-1,3-thiazol-2-yl)thio]-2-methylpropionic acid tert-butyl ester (1.72 g) synthesized in Example 293-1 was dissolved in dioxane (5 mL), 4 mol/L hydrochloric acid-dioxane (25 mL) was added, and the mixture was stirred at room temperature for 12 hr. The reaction mixture was concentrated under reduced pressure, azeotroped with diethyl ether, and the precipitated solid was collected by filtration to give the title compound (1.0 g) as a white solid.

後処理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customazeotroped with diethyl ether
  3. filtrationthe precipitated solid was collected by filtration

出典と根拠

ORDレコード
ord-ee304994f2ed4b4385f2ac823cde31d9
出典データセット
uspto-grants-2011_09
特許番号
US08026370B2

反応ノート

読み込み中…