反応 #4942

反応方程式

2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-oxazepine-5(4H)-thione

4-[bis(4-fluorophenyl)methyl]piperidine

ethanol

K2CO3

→

2-[2-[4-[Bis(4-fluorophenyl)methyl]-1-piperidinyl]ethyl]2,3-dihydro-4-methylpyrido[3,2-f][1,4]oxazepin-5(4H)-thione oxalate hydrate

反応条件

後処理

1. 1
   温度at reflux for 144 hr
2. 2
   濃縮The mixture was concentrated
3. 3
   その他the residue partitioned between chloroform and dilute sodium hydroxide
4. 4
   乾燥The chloroform was dried over anhydrous sodium sulfate
5. 5
   濃縮concentrated
6. 6
   その他The residue was chromatographed on a Waters®500 HPLC
7. 7
   洗浄eluting with absolute ethanol
8. 8
   その他The material with mass 507 was collected
9. 9
   濃縮concentrated
10. 10
    その他The residue (6 g) was reacted with 1.2 g of oxalic acid in ethanol

実験手順

A solution of 4 g (0.016 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-oxazepine-5(4H)-thione and 4.5 g (0.016 mole) of 4-[bis(4-fluorophenyl)methyl]piperidine in 100 ml of ethanol was refluxed for 48 hr. One gram of K2CO3 was added and this mixture stirred at reflux for 144 hr. The mixture was concentrated and the residue partitioned between chloroform and dilute sodium hydroxide. The chloroform was dried over anhydrous sodium sulfate and concentrated. The residue was chromatographed on a Waters®500 HPLC using a silica column and eluting with absolute ethanol. The material with mass 507 was collected and concentrated. The residue (6 g) was reacted with 1.2 g of oxalic acid in ethanol. Yield was 5 g, m.p. 125°-138° C.

出典