Water → HCID 67465258, compound

HRID 1620018Notes

Reaction equation

HRID 1620018 reaction equation
Cl[C:2]1[N:7]=[N:6][C:5]([C:8]2[CH:21]=[CH:20][C:11]3[N:12]=[C:13]([C:15]4[S:16][CH:17]=[CH:18][CH:19]=4)[O:14][C:10]=3[CH:9]=2)=[CH:4][CH:3]=1.C([O-])(=[O:24])C.[Na+].O>C(O)(=O)C>[S:16]1[CH:17]=[CH:18][CH:19]=[C:15]1[C:13]1[O:14][C:10]2[CH:9]=[C:8]([C:5]3[CH:4]=[CH:3][C:2](=[O:24])[NH:7][N:6]=3)[CH:21]=[CH:20][C:11]=2[N:12]=1

Participants

5

Reactant 3

HCID 962WaterHCID 517045Sodium AcetateHCID 86689079HCID 86689079, compound

Product 1

HCID 67465258HCID 67465258, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Conditions

Temperature
120 °C

Procedure

550 mg (1.75 mmol) 6-(6-chloro-pyridazin-3-yl)-2-thiophen-2-yl-benzoxazole in 15 mL glacial acetic acid are placed under protective gas in a pressurised vessel, 173 mg (2.11 mmol) sodium acetate are added and the mixture is stirred for 4 days at 120° C. The reaction mixture is combined with H2O and extracted with DCM. The solv. of the org. phase is eliminated i.V. The residue is suspended in ACN and a solid is suction filtered. The solid is suspended in DCM, stirred for 2 h at RT and suction filtered again.

Workup

  1. extractionextracted with DCM
  2. filtrationfiltered
  3. stirringstirred for 2 h at RT
  4. filtrationsuction filtered again

Sources & evidence

ORD record
ord-818917c4291341569c78c63627e13ea1
Source dataset
uspto-grants-2014_07
Patent number
US08772323B2

Reaction notes

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