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

HRID 442147ノート

反応式

HRID 442147 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. m.p. 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

出典と根拠

ORDレコード
ord-60e519483f104fe9bede626c85ac2e03
出典データセット
uspto-grants-1977_08
特許番号
US04044138

反応ノート

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