Piperidine → HCID 53884104、化合物

HRID 619328ノート

反応式

HRID 619328 の反応式
[Br:1][C:2]1[C:3]([OH:11])=[C:4]([OH:10])[CH:5]=[C:6]([CH:9]=1)[CH:7]=O.[S:12]([CH2:18][C:19]#[N:20])([CH2:15][C:16]#[N:17])(=[O:14])=[O:13].N1CCCCC1>C(O)C>[Br:1][C:2]1[CH:9]=[C:6]([CH:7]=[C:15]([C:16]#[N:17])[S:12]([CH2:18][C:19]#[N:20])(=[O:14])=[O:13])[CH:5]=[C:4]([OH:10])[C:3]=1[OH:11]

参加物

5

反応物 3

HCID 8082PiperidineHCID 854055-Bromo-3,4-dihydroxybenzaldehydeHCID 142163Sulphonyl diacetonitrile

生成物 1

HCID 53884104HCID 53884104、化合物収率 6.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 500 mg of 5-bromo-3,4-dihydroxybenzaldehyde and 700 mg of sulfonly diacetonitrile in 6 ml of ethanol was refluxed with few drops of piperidine for 4 hours. Ethanol was removed in rotavap and the mixture worked up with ethyl acetate, diluted acid and brine. A portion of the crude was then purified by HPLC on a C-18 column to provide about 50 mg of 2-(3-bromo-4,5-dihydroxyphenyl)-1-cyano-1-cyanomethylsulfonly ethene.

後処理

  1. customEthanol was removed in rotavap
  2. additiondiluted acid and brine
  3. customA portion of the crude was then purified by HPLC on a C-18 column

出典と根拠

ORDレコード
ord-7ce82f49b6b4482482eee56e659a480c
出典データセット
uspto-grants-1999_09
特許番号
US05958959

反応ノート

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