Oxalic acid dihydrate → 3-Methyl-5,6,7,8-tetrahydroquinoline-8-thiocarboxamide oxalate

HRID 437470ノート

反応式

HRID 437470 の反応式
[CH3:1][C:2]1[CH:3]=[N:4][C:5]2[CH:6]([C:12](=[S:14])[NH2:13])[CH2:7][CH2:8][CH2:9][C:10]=2[CH:11]=1.O.O.[C:17]([OH:22])(=[O:21])[C:18]([OH:20])=[O:19]>C(O)C>[C:17]([OH:22])(=[O:21])[C:18]([OH:20])=[O:19].[CH3:1][C:2]1[CH:3]=[N:4][C:5]2[CH:6]([C:12](=[S:14])[NH2:13])[CH2:7][CH2:8][CH2:9][C:10]=2[CH:11]=1

参加物

4

反応物 2

HCID 61373Oxalic acid dihydrateHCID 30039215,6,7,8-Tetrahydro-3-methyl-8-quinolinecarbothioamide

生成物 1

HCID 203583943-Methyl-5,6,7,8-tetrahydroquinoline-8-thiocarboxamide oxalate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of 3-methyl-5,6,7,8-tetrahydroquinoline-8-thiocarboxamide (1 g.) in hot ethanol (10 ml.) was added a solution of oxalic acid dihydrate (650 mg.) in hot ethanol (6.5 ml.). The solution was filtered and allowed to cool when the oxalate crystallised. The oxalate was removed by filtration, washed with ether and dried. Yield 1 g. 186°-8° C. Found: C, 52.71%; H, 5.63%; N, 9.19%. Calc. for C13H16N2O4S : C, 52.70%; H, 5.44%; N, 9.46%.

後処理

  1. filtrationThe solution was filtered
  2. temperatureto cool when the oxalate
  3. customcrystallised
  4. customThe oxalate was removed by filtration
  5. washwashed with ether
  6. customdried
  7. custom186°-8° C

出典と根拠

ORDレコード
ord-a7c81952c2f243e0821326c435d06959
出典データセット
uspto-grants-1977_06
特許番号
US04031102

反応ノート

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