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3-Cyclobutene-1,2-dione, 3,4-dimethoxy- → HCID 21423011、化合物

HRID 259076
ノート
印刷プレビュー

反応式

HRID 259076 の反応式
[CH2:1]([N:4]1[CH2:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1)[CH2:2][CH3:3].CO[C:13]1[C:14](=O)[C:15](=[O:19])[C:16]=1[O:17]C>CO>[CH2:1]([N:4]1[CH2:10][CH2:9][CH2:8][N:7]([C:13]2[C:16](=[O:17])[C:15](=[O:19])[C:14]=2[N:7]2[CH2:8][CH2:9][CH2:10][N:4]([CH2:1][CH2:2][CH3:3])[CH2:5][CH2:6]2)[CH2:6][CH2:5]1)[CH2:2][CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 1232273-Cyclobutene-1,2-dione, 3,4-dimethoxy-HCID 122617971-Propyl-1,4-diazepane

生成物 1

HCID 21423011HCID 21423011、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

A solution of 3.1 grams of 1-propylhomopiperazine in 20 ml. of methanol is mixed with a solution of 1.6 grams of 3,4-dimethoxy-3-cyclobutene-1,2-dione in 50 ml. of methanol and refluxed under nitrogen for 5 hours. The methanol solvent is evaporated by heating on a steam bath and the residual solid is dissolved in 70 ml. of anhydrous benzene at room temperature, treated with charcoal, and filtered. The resulting filtrate is diluted with 250 ml. of hexane and the precipitate which forms is separated by filtration and dried and then recrystallized from 1000 ml. of refluxing hexane to give 3,4-bis(4-propyl-1-homopiperazinyl)-3-cyclobutene-1,2-dione as white crystals melting at about 90°-92° C.

後処理

  1. customThe methanol solvent is evaporated
  2. temperatureby heating on a steam bath
  3. dissolutionthe residual solid is dissolved in 70 ml
  4. additionof anhydrous benzene at room temperature, treated with charcoal
  5. filtrationfiltered
  6. additionThe resulting filtrate is diluted with 250 ml
  7. customof hexane and the precipitate which forms is separated by filtration
  8. customdried
  9. customrecrystallized from 1000 ml

出典と根拠

ORDレコード
ord-e65694aedc844750a977ffe2dcb6d116
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04036828

反応ノート

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