1,4-Dioxane hydrochloride → HCID 178473770、化合物

HRID 13347

反応式

HRID 13347 の反応式
[CH3:1][S:2]([C:5]1[CH:37]=[CH:36][C:8]([O:9][C:10]2[C:11]([CH:24]3[CH2:28][CH2:27][CH2:26][N:25]3[C:29]([O:31]C(C)(C)C)=O)=[CH:12][C:13]3[NH:17][C:16]([C:18]4[CH:22]=[CH:21][NH:20][N:19]=4)=[N:15][C:14]=3[CH:23]=2)=[CH:7][CH:6]=1)(=[O:4])=[O:3].Cl.O1CCOC[CH2:40]1>>[CH3:1][S:2]([C:5]1[CH:37]=[CH:36][C:8]([O:9][C:10]2[C:11]([CH:24]3[CH2:28][CH2:27][CH2:26][N:25]3[C:29](=[O:31])[CH3:40])=[CH:12][C:13]3[NH:17][C:16]([C:18]4[CH:22]=[CH:21][NH:20][N:19]=4)=[N:15][C:14]=3[CH:23]=2)=[CH:7][CH:6]=1)(=[O:3])=[O:4]

参加物

3

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 178451667HCID 178451667、化合物

生成物 1

HCID 178473770HCID 178473770、化合物

実験手順

49.2 mg of t-butyl 2-(6-(4-methanesulfonyl-phenoxy)-2-(1H-pyrazol-3-yl)-3H-benzimidazol-5-yl)-pyrrolidin-1-carboxylate was dissolved in 1 ml of 4 N hydrochloric acid-dioxane, and the reaction liquid was stirred at room temperature for 2 hours. The reaction solvent was evaporated away under reduced pressure, and 0.012 ml of acetic anhydride was added to 2 ml of a pyridine solution of the resulting residue, and stirred at room temperature for 30 minutes. The reaction solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=9/1) to obtain the entitled compound as a brown solid.

後処理

  1. customthe reaction liquid
  2. customThe reaction solvent was evaporated away under reduced pressure, and 0.012 ml of acetic anhydride
  3. additionwas added to 2 ml of a pyridine solution of the resulting residue
  4. stirringstirred at room temperature for 30 minutes
  5. customThe reaction solvent was evaporated away under reduced pressure
  6. customthe resulting residue was purified
  7. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=9/1)

出典と根拠

ORDレコード
ord-b595d5b9f8fc487e894252a68159e07e
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

関連ノート

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