تفاعل #2271666

معادلة التفاعل

α-chloro-2-bromobenzaldehyde phenylsulfonylhydrazone

N-methylpiperazine

→

brown gum

المردود 124.8%

1[[(Phenylsulfonyl)hydrazono]-(2- bromophenyl)methyl]-4-methylpiperazine

المردود 124.8%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   workup.WAITto stand at ambient temperature for 16 hours
2. 2
   درجة الحرارةThe reaction was chilled in an ice bath
3. 3
   ترشيحfiltered
4. 4
   أخرىto remove the piperazine hydrochloride that
5. 5
   أخرىwas formed
6. 6
   تركيزThe filtrate was concentrated
7. 7
   أخرىto yield a brown gum
8. 8
   أخرىThe gum was triturated with hot acetonitrile
9. 9
   درجة الحرارةthe mixture was cooled in an ice bath
10. 10
    ترشيحwhen cold, was filtered
11. 11
    أخرىto remove unwanted side product
12. 12
    تركيزThe filtrate was then concentrated

الإجراء التجريبي

To a stirred solution, under nitrogen, of α-chloro-2-bromobenzaldehyde phenylsulfonylhydrazone (271.1 g, 720 mmol) in tetrahydrofuran (THF; 2 L), was added dropwise N-methylpiperazine (159.7 g; 1600 mmol). The reaction was stirred at ambient temperature for three hours, and then permitted to stand at ambient temperature for 16 hours. The reaction was chilled in an ice bath, and then filtered to remove the piperazine hydrochloride that was formed. The filtrate was concentrated to yield a brown gum. The gum was triturated with hot acetonitrile, the mixture was cooled in an ice bath, and when cold, was filtered to remove unwanted side product. The filtrate was then concentrated to afford 392.9 g of a brown gum of crude 1-[[(phenylsulfon-yl)hydrazono]-(2-bromophenyl)methyl]-4-methylpiperazine.

المصدر