(Diethylamino)sulfur trifluoride → HCID 178461108, 화합물

HRID 13364

반응식

HRID 13364 반응식
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]

참가 물질

5

반응물 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

생성물 1

HCID 178461108HCID 178461108, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
-78 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-24f8fe4802174c569b9c21dcebe30083
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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