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Ethanol → 3H-Indeno(1,2-c)pyridazin-3-one, 2,4,4a,5-tetrahydro-7-amino-

HRID 845058
ノート
印刷プレビュー

反応式

HRID 845058 の反応式
C([NH:4][C:5]1[CH:6]=[C:7]2[C:16](=[CH:17][CH:18]=1)[C:10]1=[N:11][NH:12][C:13](=[O:15])[CH2:14][CH:9]1[CH2:8]2)(=O)C.C(O)C>O.NN>[NH2:4][C:5]1[CH:6]=[C:7]2[C:16](=[CH:17][CH:18]=1)[C:10]1=[N:11][NH:12][C:13](=[O:15])[CH2:14][CH:9]1[CH2:8]2
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 702EthanolHCID 13603296103422-54-4

生成物 1

HCID 3579973H-Indeno(1,2-c)pyridazin-3-one, 2,4,4a,5-tetrahydro-7-amino-収率 33%

試薬・触媒・溶媒 1

HCID 24654Hydrazine hydrate (1:1)溶媒

実験手順

7-Acetamido-4,4a-dihydro-[5H]-indeno[1,2-c]pyridazin-3[2H]-one (1.50 g) was suspended in hydrazine hydrate (30 ml ) and heated under reflux with ethanol (5 ml ) for 2 hours. The solution was filtered through diatomaceous earth, allowed to cool, then extracted into chloroform. The combined organic extracts were dried over magnesium sulphate and concentrated. Recrystallisation of the crude product from n-propanol gave 7-amino-4,4a-dihydro-[5H]-indeno[1,2-c]pyridazin-3[2H]-one (0.41 g, m.p. 244°-245° C.) as a pale yellow powder; ν(Nujol mull) 3400, 3320, 3220, 1652, 1635, 1600, and 1580cm-1 ; δ(DMSO-d6) 2.50 (3H,m,4-H,5-H2), 3.05 (1H,m,4a-H), 5.67 (2H,s(br),NH2), 6.55 (2H,m,6,H-H), 7.27 (1H,d,9-H).

後処理

  1. temperatureheated
  2. filtrationThe solution was filtered through diatomaceous earth
  3. temperatureto cool
  4. extractionextracted into chloroform
  5. dry with materialThe combined organic extracts were dried over magnesium sulphate
  6. concentrationconcentrated
  7. customRecrystallisation of the crude product from n-propanol

出典と根拠

ORDレコード
ord-22cc40852bda433eb02bebe7aea728c0
出典データセット
uspto-grants-1988_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04755511

反応ノート

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