Ammonia → HCID 86583938, compound

HRID 1782705Notes

Reaction equation

HRID 1782705 reaction equation
[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]2[CH2:16][C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[NH:9][C:8]2=[O:17])[CH2:3][CH2:2]1.[C:18]([O-:21])(=[O:20])[CH3:19].[H][H].ClCCl.CO.N>CO.[Rh+]=O.O.[Pt](=O)=O>[NH:1]1[CH2:6][CH2:5][CH:4]([N:7]2[CH2:16][CH:15]3[CH:10]([CH2:11][CH2:12][CH2:13][CH2:14]3)[NH:9][C:8]2=[O:17])[CH2:3][CH2:2]1.[C:18]([O-:21])(=[O:20])[CH3:19]

Participants

7

Reactant 4

HCID 222AmmoniaHCID 21226129Dichloromethane methanolHCID 86583939HCID 86583939, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 86583938HCID 86583938, compound

Reagents, catalysts & solvents 2

HCID 178526986HCID 178526986, compoundCatalystHCID 887MethanolSolvent

Procedure

A solution of 5.0 g (17.17 mmol) of 3,4-dihydro-3-(4-piperidinyl)-2(1H)-quinazolinone-acetate in 70 ml of methanol was hydrogenated at room temperature and in the presence of 1.0 g rhodium (III) oxide-platinum (IV) oxide hydrate catalyst (46.45% rhodium, 20.15% platinum) until the hydrogen uptake had ceased. The catalyst and solvent were removed, the residue was triturated with 10 ml of diisopropylether and a few drops of isopropanol and the resulting crystals were suction filtered. After drying in vacuo 4.4 g (86.2% of theory) of colourless crystals were obtained, Rf=0.3 (eluant: dichloromethane/methanol/conc. ammonia 7.5/2.5/0.5 v/v/v).

Workup

  1. customThe catalyst and solvent were removed
  2. customthe residue was triturated with 10 ml of diisopropylether and a few drops of isopropanol
  3. customAfter drying in vacuo 4.4 g (86.2% of theory) of colourless crystals
  4. customwere obtained

Sources & evidence

ORD record
ord-c77a00f1f4914724b3abd5bbcc00f5e6
Source dataset
uspto-grants-2009_03
Patent number
US07498325B2

Reaction notes

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