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

HRID 259072

반응식

HRID 259072 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7410d28cffb0491395fb23b9c4298dfe
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04036828

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