Methanol → HCID 86619215, compound

HRID 13404Notes

Reaction equation

HRID 13404 reaction equation
C(=O)([O-])[O-].[K+].[K+].CO.C([O:12][CH2:13][C:14]([N:16]1[CH2:20][CH2:19][CH2:18][CH:17]1[C:21]1[C:22]([O:36][C:37]2[CH:42]=[CH:41][C:40]([C:43]3[CH:48]=[CH:47][CH:46]=[CH:45][C:44]=3[F:49])=[CH:39][CH:38]=2)=[CH:23][C:24]2[N:28]=[C:27]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=3)[NH:26][C:25]=2[CH:35]=1)=[O:15])(=O)C>C(Cl)(Cl)Cl>[F:49][C:44]1[CH:45]=[CH:46][CH:47]=[CH:48][C:43]=1[C:40]1[CH:39]=[CH:38][C:37]([O:36][C:22]2[C:21]([CH:17]3[CH2:18][CH2:19][CH2:20][N:16]3[CH:14]([OH:15])[CH:13]=[O:12])=[CH:35][C:25]3[NH:26][C:27]([C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=4)=[N:28][C:24]=3[CH:23]=2)=[CH:42][CH:41]=1

Participants

5

Reactant 3

HCID 887MethanolHCID 11430Potassium CarbonateHCID 67482967HCID 67482967, compound

Product 1

HCID 86619215HCID 86619215, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

10 mg of potassium carbonate was added to a methanol (0.5 ml) solution of 11 mg of 2-(2-(5-((2′-fluorobiphenyl-4-yl)oxy)-2-pyridin-2-yl-1H-benzimidazol-6-yl)pyrrolidin-1-yl)-2-oxoethyl acetate obtained in Example 513, and the reaction liquid was stirred at room temperature for 1 day. The reaction liquid was diluted with chloroform, washed with water and saturated saline in order, and dried with anhydrous sodium sulfate. The 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=10/1) to obtain the entitled compound as a white solid.

Workup

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. washwashed with water and saturated saline in order
  4. dry with materialdried with anhydrous sodium sulfate
  5. customThe 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=10/1)

Sources & evidence

ORD record
ord-5143ed0d00a745448befe40ede8bdf1a
Source dataset
uspto-grants-2010_06
Patent number
US07728025B2

Reaction notes

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