7-BENZYL-5,6,7,8-TETRAHYDRO4-CHLORO-PYRIDO[3,4-D]PYRIMIDINE HYDROCHLORIDE synthesis
- Product Name:7-BENZYL-5,6,7,8-TETRAHYDRO4-CHLORO-PYRIDO[3,4-D]PYRIMIDINE HYDROCHLORIDE
- CAS Number:192869-80-0
- Molecular formula:C14H14ClN3
- Molecular Weight:259.73
![7-BENZYL-5,6,7,8-TETRAHYDRO-3H-PYRIDO[3,4-D]PYRIMIDIN-4-ONE HYDROCHLORIDE](/CAS/GIF/62458-96-2.gif)
62458-96-2
139 suppliers
$16.00/250mg
192869-80-0
107 suppliers
$43.00/1g
Yield: 100%
Reaction Conditions:
Stage #1:7-benzyl-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-4(3H)-one with N-ethyl-N,N-diisopropylamine;trichlorophosphate in toluene at 100; for 0.5 h;
Stage #2: with sodium hydrogencarbonate in water;toluene at 20; for 1 h;
Steps:
69.B
To 69A (3.00 g, 12.4 mmol) in toluene (40 mL) at room temperature was added phosphorus oxychloride (2.28 g, 14.9 mmol) followed by Hunig's base (1.28 g, 9.92 mmol) and the reaction was heated to 100°C for 30 minutes then cooled to rt. The resulting mixture was quenched with 200 mL of saturated aqueous sodium bicarbonate solution and 200 mL of crushed ice. After stirring at room temperature for lh, the mixture was then extracted with dichloromethane (100 mL x 4). The combined organic extracts were dried over sodium sulfate and concentrated in vacuo to give 3.32 g of 69B (-100%) as a dark brown oil that was used directly without any further purification. HPLC Ret. Time: 0.95 min. MH+ (m/z) 260.
References:
Location in patent:Page/Page column 86
![Pyrido[3,4-d]pyriMidin-4(1H)-one, 5,6,7,8-tetrahydro-7-(phenylMethyl)-, Monohydrochloride](/CAS/GIF/69981-00-6.gif)
69981-00-6
11 suppliers
$273.48/1g
192869-80-0
107 suppliers
$43.00/1g
62458-96-2
139 suppliers
$16.00/250mg
192869-80-0
107 suppliers
$43.00/1g
6313-33-3
199 suppliers
$9.00/1g
52763-21-0
245 suppliers
$6.00/1g
192869-80-0
107 suppliers
$43.00/1g
52763-21-0
245 suppliers
$6.00/1g
192869-80-0
107 suppliers
$43.00/1g