反応 #2383814

反応方程式

Triphenylphosphine

product

6,7,8,9-tetrahydro-5-(hydroxymethyl)-3H,5H-[1,2,4]oxadiazolo[4,3-a]azepin-3-one

carbon tetrabromide

→

title compound

5-(bromomethyl)-6,7,8,9-tetrahydro-3H,5H-[1,2,4]oxadiazolo[4,3-a]azepin-3-one

溶媒

dichloromethane

反応条件

後処理

1. 1
   温度This solution was cooled in an ice bath
2. 2
   workup.STIRRINGstirring
3. 3
   workup.WAITwas continued for 5 minutes at 0° C.
4. 4
   その他The solvent was removed under reduced pressure
5. 5
   ろ過a filter
6. 6
   洗浄washed three times with ether
7. 7
   その他The filtrate solvent was then removed under reduced pressure

実験手順

To a solution of the product of Example 5 in dichloromethane was added carbon tetrabromide (460 mg, 1.3 mmol). This solution was cooled in an ice bath and stirred for 5 minutes. Triphenylphosphine (437 mg, 1.6 mmol) was added to the solution and stirring was continued for 5 minutes at 0° C. before allowing it to warm slowly to room temperature. The solvent was removed under reduced pressure. The residue was placed on a filter and washed three times with ether. The filtrate solvent was then removed under reduced pressure to yield the title compound. Mass Spectra for C8H11N2O2Br: M+H=246.

出典