(Diethylamino)sulfur trifluoride → HCID 178461108、化合物

HRID 13364

反応式

HRID 13364 の反応式
C(N(S(F)(F)[F:7])CC)C.[CH3:10][S:11]([C:14]1[CH:43]=[CH:42][C:17]([O:18][C:19]2[C:20]([N:34]3[CH2:38][CH2:37][CH2:36][CH:35]3[CH:39](O)[CH3:40])=[CH:21][C:22]3[NH:26][C:25]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=4)=[N:24][C:23]=3[CH:33]=2)=[CH:16][CH:15]=1)(=[O:13])=[O:12].C(=O)(O)[O-].[Na+]>C(Cl)(Cl)Cl>[F:7][CH:39]([CH:35]1[CH2:36][CH2:37][CH2:38][N:34]1[C:20]1[C:19]([O:18][C:17]2[CH:42]=[CH:43][C:14]([S:11]([CH3:10])(=[O:13])=[O:12])=[CH:15][CH:16]=2)=[CH:33][C:23]2[NH:24][C:25]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][N:28]=3)=[N:26][C:22]=2[CH:21]=1)[CH3:40]

参加物

5

反応物 3

HCID 123472(Diethylamino)sulfur trifluorideHCID 516892Sodium BicarbonateHCID 231453781-(1-(6-(4-Methanesulfonyl-phenoxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-2-yl)-ethanol

生成物 1

HCID 178461108HCID 178461108、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
-78 °C

実験手順

0.007 ml of diethylaminosulfur trifluoride was added to a chloroform (1 ml) solution of 21 mg of 1-(1-(6-(4-methanesulfonyl-phenoxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-2-yl)-ethanol diastereomer A obtained in Example 354, at −78° C., and the reaction liquid was stirred at −78° C. for 1 hour. The reaction liquid was heated up to room temperature, and aqueous saturated sodium bicarbonate was added to the reaction liquid, and then extracted with ethyl acetate, and dried with anhydrous magnesium sulfate. The solvent was evaporated away, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1) to obtain the entitled compound as a pale yellow solid.

後処理

  1. customA obtained in Example 354, at −78° C.
  2. customthe reaction liquid
  3. customThe reaction liquid
  4. temperaturewas heated up to room temperature
  5. extractionextracted with ethyl acetate
  6. dry with materialdried with anhydrous magnesium sulfate
  7. customThe solvent was evaporated away
  8. customthe resulting residue was purified
  9. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=10/1)

出典と根拠

ORDレコード
ord-24f8fe4802174c569b9c21dcebe30083
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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