1-Methylpiperazine → 3,4-Bis(4-methylpiperazin-1-yl)cyclobut-3-ene-1,2-dione

HRID 259072

反応式

HRID 259072 の反応式
CO[C:3]1[C:4](=O)[C:5](=[O:9])[C:6]=1[O:7]C.[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1>C(O)C>[CH3:11][N:12]1[CH2:17][CH2:16][N:15]([C:3]2[C:6](=[O:7])[C:5](=[O:9])[C:4]=2[N:15]2[CH2:16][CH2:17][N:12]([CH3:11])[CH2:13][CH2:14]2)[CH2:14][CH2:13]1

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 1232273-Cyclobutene-1,2-dione, 3,4-dimethoxy-

生成物 1

HCID 214230243,4-Bis(4-methylpiperazin-1-yl)cyclobut-3-ene-1,2-dione

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A solution of 1.0 gram of 3,4-dimethoxy-3-cyclobutene-1,2-dione dissolved in 30 ml. of absolute ethanol is mixed with a solution of 1.4 grams of 1-methylpiperazine in 30 ml. of absolute ethanol. The resulting mixture is stirred and heated to reflux for 5 hours under an atmosphere of dry nitrogen. After concentration to approximately one-sixth the volume under reduced pressure, the reaction mixture is cooled and crystallization is induced by scratching. The resultant precipitate is filtered, washed with 0.5 ml. of absolute ethanol, and dried in a steam cabinet. The resulting, product, 3,4-bis(4-methyl-1-piperazinyl)-3-cyclobutene-1,2-dione is obtained as white crystals melting at about 189°-191° C.

後処理

  1. temperatureheated
  2. temperatureto reflux for 5 hours under an atmosphere of dry nitrogen
  3. concentrationAfter concentration to approximately one-sixth the volume under reduced pressure
  4. temperaturethe reaction mixture is cooled
  5. customcrystallization
  6. filtrationThe resultant precipitate is filtered
  7. washwashed with 0.5 ml
  8. dry with materialof absolute ethanol, and dried in a steam cabinet

出典と根拠

ORDレコード
ord-7410d28cffb0491395fb23b9c4298dfe
出典データセット
uspto-grants-1977_07
特許番号
US04036828

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