1,4-Dioxane hydrochloride → 2-(4-{[(3,4-Dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-4-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)methyl]-1,3-thiazole-5-carboxylic acid

HRID 2234010ノート

反応式

HRID 2234010 の反応式
[C:1]([C:4]1[CH:38]=[CH:37][CH:36]=[CH:35][C:5]=1[C:6]([NH:8][CH2:9][C:10]1[N:11]=[C:12]([N:18]2[CH2:23][CH2:22][CH:21]([NH:24][C:25]([C:27]3[NH:28][C:29]([CH3:34])=[C:30]([Cl:33])[C:31]=3[Cl:32])=[O:26])[CH2:20][CH2:19]2)[S:13][C:14]=1[C:15]([OH:17])=[O:16])=[O:7])([OH:3])=O.Cl.O1CCOCC1>>[Cl:32][C:31]1[C:30]([Cl:33])=[C:29]([CH3:34])[NH:28][C:27]=1[C:25]([NH:24][CH:21]1[CH2:22][CH2:23][N:18]([C:12]2[S:13][C:14]([C:15]([OH:17])=[O:16])=[C:10]([CH2:9][N:8]3[C:6](=[O:7])[C:5]4[C:4](=[CH:38][CH:37]=[CH:36][CH:35]=4)[C:1]3=[O:3])[N:11]=2)[CH2:19][CH2:20]1)=[O:26]

参加物

3

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 68581174HCID 68581174、化合物

生成物 1

HCID 685796992-(4-{[(3,4-Dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-4-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)methyl]-1,3-thiazole-5-carboxylic acid収率 32.4%

実験手順

4-{[(2-Carboxybenzoyl)amino]methyl}-2-(4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-1,3-thiazole-5-carboxylic acid (Example 244; 100 mg; 0.17 mmol) was stirred with 4 N HCl/Dioxane (3 ml) at room temperature for 8 h. The mixture was concentrated in vacuo and the resulting solid was purified by reversed phase HPLC eluting with water/acetonitrile/ammonium acetate buffer mixtures giving the title compound (31 mg).

後処理

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe resulting solid was purified by reversed phase HPLC
  3. washeluting with water/acetonitrile/ammonium acetate buffer mixtures

出典と根拠

ORDレコード
ord-fa7f709dd7a04f43aad1666b558fafd6
出典データセット
uspto-grants-2010_05
特許番号
US07709503B2

反応ノート

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