Ethanol → HCID 178505885, compound

HRID 13250Notes

Reaction equation

HRID 13250 reaction equation
[C:1](=[S:3])=S.[OH-].[K+].C(O)C.[F:9][C:10]1[CH:38]=[CH:37][C:13]([O:14][C:15]2[C:23]3[N:22]=C(C4C=CC=CN=4)[NH:20][C:19]=3[CH:18]=[C:17]([O:30][C:31]3[CH:32]=[N:33][CH:34]=[CH:35][CH:36]=3)[CH:16]=2)=[CH:12][CH:11]=1>C(OCC)(=O)C>[F:9][C:10]1[CH:38]=[CH:37][C:13]([O:14][C:15]2[C:23]3[N:22]=[C:1]([SH:3])[NH:20][C:19]=3[CH:18]=[C:17]([O:30][C:31]3[CH:32]=[N:33][CH:34]=[CH:35][CH:36]=3)[CH:16]=2)=[CH:12][CH:11]=1

Participants

6

Reactant 4

HCID 702EthanolHCID 6348Carbon DisulfideHCID 14797Potassium HydroxideHCID 231452784-(4-Fluoro-phenoxy)-2-pyridin-2-yl-6-(pyridin-3-yloxy)-1H-benzimidazole

Product 1

HCID 178505885HCID 178505885, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Conditions

Temperature
80 °C

Procedure

0.06 ml of carbon disulfide and 54 mg of potassium hydroxide were added to an ethanol (2.0 ml) solution of 273 mg of 3-(4-fluoro-phenoxy)-5-(pyridin-3-yloxy)-benzene-1,2-diamine obtained in Example 68, and the reaction liquid was stirred overnight at 80° C. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline in order, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure to obtain the entitled compound.

Workup

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. washwashed with water and saturated saline in order
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customThe solvent was evaporated away under reduced pressure
  6. customto obtain the entitled compound

Sources & evidence

ORD record
ord-bb729575983b44119b5762c8c620b5c4
Source dataset
uspto-grants-2010_06
Patent number
US07728025B2

Reaction notes

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