p-Toluenesulfonic acid → HCID 53642864、化合物

HRID 1438699ノート

反応式

HRID 1438699 の反応式
[CH3:1][N:2]1[C:7](=[O:8])[NH:6][CH:5]([S:9][CH3:10])[N:4]([N:11]=C(C)C)[C:3]1=[O:15].C1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)C>[CH3:1][N:2]1[C:7](=[O:8])[NH:6][CH:5]([S:9][CH3:10])[N:4]([NH2:11])[C:3]1=[O:15]

参加物

4

反応物 2

HCID 6101p-Toluenesulfonic acidHCID 53804495HCID 53804495、化合物

生成物 1

HCID 53642864HCID 53642864、化合物収率 96%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

22.8 g (0.1 mole) of 1-methyl-3-isopropylideneamino-4-methylmercapto-tetrahydro-1,3,5-triazine-2,6-dione (prepared according to Example 1) were dissolved in 250 ml of ethanol and warmed, with addition of a pinch of p-toluene-sulphonic acid, for 5 hours to 50° C, whilst applying a vacuum of about 200 mm Hg. The mixture was evaporated in vacuo and the residue was recrystallized from ethanol. 18 g (96%) of 1-methyl3-amino-4-methylmercapto-tetrahydro-1,3,5-triazine-2,6-dione were obtained as colorless needles; melting point 174°-175° C.

後処理

  1. customThe mixture was evaporated in vacuo
  2. customthe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-9d499fb7000b4a3bbae9377699672e6d
出典データセット
uspto-grants-1977_11
特許番号
US04056527

反応ノート

読み込み中…