HCID 59443036, compound → HCID 59443017, compound

HRID 1959143Notes

Reaction equation

HRID 1959143 reaction equation
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([NH:18]C(=O)OC(C)(C)C)=[CH:15][CH:16]=3)[O:11][C:10]([CH3:27])([CH3:26])[CH:9]=2)=[CH:4][CH:3]=1>Cl.ClCCl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([NH2:18])=[CH:15][CH:16]=3)[O:11][C:10]([CH3:27])([CH3:26])[CH:9]=2)=[CH:4][CH:3]=1

Participants

3

Reactant 1

HCID 59443036HCID 59443036, compound

Product 1

HCID 59443017HCID 59443017, compound

Reagents, catalysts & solvents 1

HCID 19696284HCl dichloromethaneSolvent

Procedure

A mixture of the compound obtained in (4) described above (2.8 g) and 2M hydrochloric acid-dichloromethane solution (100 mL) was stirred at room temperature overnight. The reaction mixture was washed successively with a saturated aqueous solution of sodium bicarbonate and brine, dried over sodium sulfate and concentrated in vacuo. The residue is purified by flush chromatography on silica gel (Solvent; petroleum ether/ethyl acetate=25/1) to give the titled compound (1.9 g) as a yellow powder.

Workup

  1. additionA mixture of the compound
  2. washThe reaction mixture was washed successively with a saturated aqueous solution of sodium bicarbonate and brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue is purified
  6. customby flush chromatography on silica gel (Solvent; petroleum ether/ethyl acetate=25/1)

Sources & evidence

ORD record
ord-83a6a2fd37ba4fa8bac8f25338b8625b
Source dataset
uspto-grants-2013_04
Patent number
US08410166B2

Reaction notes

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