HCID 86671245, compound → HCID 68526231, compound

HRID 884138Notes

Reaction equation

HRID 884138 reaction equation
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([NH:21][C:22](=[O:31])[C:23]3[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([Cl:30])[CH:24]=3)=[CH:17][N:16]=2)=[CH:10][CH:9]=1)(C)(C)C>C(Cl)(Cl)Cl.CO.C(OCC)(=O)C>[ClH:29].[ClH:29].[NH2:7][C:8]1[CH:13]=[CH:12][C:11]([O:14][C:15]2[N:16]=[CH:17][C:18]([NH:21][C:22](=[O:31])[C:23]3[CH:28]=[CH:27][C:26]([Cl:29])=[C:25]([Cl:30])[CH:24]=3)=[CH:19][CH:20]=2)=[CH:10][CH:9]=1

Participants

3

Reactant 1

HCID 86671245HCID 86671245, compound

Product 1

HCID 68526231HCID 68526231, compound

Reagents, catalysts & solvents 1

HCID 21956348HCID 21956348, compoundSolvent

Procedure

t-Butyl{4-[5-(3,4-dichlorobenzoylamino)-pyridin-2-yloxy]phenyl}carbamate (4.31 g, 9.09 mmol) was dissolved in a mixed solution of chloroform-methanol-ethyl acetate. The resulting solution was concentrated to a volume of about 20 mL. To the residue solution was added a solution of 4 N hydrogen chloride in ethyl acetate (70 mL), and left to cool for 2 hours at room temperature. The precipitated white powder was filtered, and washed with ethyl acetate, to thereby yield 4.04 g of the title compound.

Workup

  1. concentrationThe resulting solution was concentrated to a volume of about 20 mL
  2. additionTo the residue solution was added a solution of 4 N hydrogen chloride in ethyl acetate (70 mL)
  3. waitleft
  4. filtrationThe precipitated white powder was filtered
  5. washwashed with ethyl acetate

Sources & evidence

ORD record
ord-152ba46af7e3463e827463b53ece5dee
Source dataset
uspto-grants-2012_08
Patent number
US08236826B2

Reaction notes

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