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Acetic Acid → 5,6-Dimethoxy-3[4(2-methylpropyloxycarbonyl)piperazino]methylene oxindole

HRID 47071
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HRID 47071 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[NH:8][C:7](=[O:14])[C:6]2=[CH:15]O.C(O)(=O)C.[CH2:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1)=[O:27])[CH:22]([CH3:24])[CH3:23]>C1C=CC=CC=1.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[NH:8][C:7](=[O:14])[C:6]2=[CH:15][N:31]1[CH2:30][CH2:29][N:28]([C:26]([O:25][CH2:21][CH:22]([CH3:24])[CH3:23])=[O:27])[CH2:33][CH2:32]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 11788701Isobutyl piperazine-1-carboxylateHCID 178486553HCID 178486553, 화합물

생성물 1

HCID 539513465,6-Dimethoxy-3[4(2-methylpropyloxycarbonyl)piperazino]methylene oxindole

시약·촉매·용매 2

HCID 241Benzene용매2회HCID 962Water
용매

실험 절차

5.00 g. of 5,6-Dimethoxy-3-hydroxymethylene oxindole, 2.5 g. acetic acid and 6.5 g. piperazine-N-carboxylic acid isobutyl ester (U.S. Pat. No. 3,635,979) in 40 ml. benzene was refluxed using a water separator to remove the water as it formed. After 20 minutes, 200 ml. benzene was added and the solution extracted with potassium carbonate and water. The benzene solution was treated with magnesium sulfate and charcoal, filtered, concentrated and the residue crystallized from isopropyl alcohol and ether to give 5.50 g. product, m.p. 195°-197° C.

후처리

  1. customto remove the water as it
  2. customformed
  3. extractionthe solution extracted with potassium carbonate and water
  4. additionThe benzene solution was treated with magnesium sulfate and charcoal
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customthe residue crystallized from isopropyl alcohol and ether
  8. customto give 5.50 g

출처 및 근거

ORD 기록
ord-72970bca4ce742a8bdfe7b556c92414c
출처 데이터셋
uspto-grants-1979_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04176191

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