1,4-Dioxane hydrochloride → HCID 178473770, 화합물

HRID 13347

반응식

HRID 13347 반응식
[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]

참가 물질

3

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 178451667HCID 178451667, 화합물

생성물 1

HCID 178473770HCID 178473770, 화합물

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-b595d5b9f8fc487e894252a68159e07e
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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