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3-Cyclobutene-1,2-dione, 3,4-dimethoxy- → HCID 21423011, 화합물

HRID 259076
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HRID 259076 반응식
[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]
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참가 물질

4

반응물 2

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

생성물 1

HCID 21423011HCID 21423011, 화합물

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e65694aedc844750a977ffe2dcb6d116
출처 데이터셋
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04036828

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