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

HRID 47071

反応式

HRID 47071 の反応式
[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

参加物

6

反応物 3

HCID 176Acetic AcidHCID 11788701Isobutyl piperazine-1-carboxylateHCID 178486553HCID 178486553、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 241Benzene溶媒2 回HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-72970bca4ce742a8bdfe7b556c92414c
出典データセット
uspto-grants-1979_11
特許番号
US04176191

関連ノート

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