Diisopropyl Ether → N-Methyl-5-(methylsulfanyl)-3-oxo-1,2,4-thiadiazole-2(3H)-carboxamide

HRID 1833813ノート

反応式

HRID 1833813 の反応式
C(N(CC)CC)C.[CH3:8][N:9]=[C:10]=[O:11].[OH:12][C:13]1[N:17]=[C:16]([S:18][CH3:19])[S:15][N:14]=1.C(OC(C)C)(C)C>O1CCCC1>[CH3:8][NH:9][C:10]([N:14]1[C:13](=[O:12])[N:17]=[C:16]([S:18][CH3:19])[S:15]1)=[O:11]

参加物

6

反応物 4

HCID 7914Diisopropyl EtherHCID 8471TriethylamineHCID 12228Methyl IsocyanateHCID 178503579HCID 178503579、化合物

生成物 1

HCID 12526283N-Methyl-5-(methylsulfanyl)-3-oxo-1,2,4-thiadiazole-2(3H)-carboxamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
20 °C

実験手順

0.1 ml of triethylamine and 5 ml of methyl isocyanate were added to a solution of 7.5 g of 3-hydroxy-5-methylthio-1,2,4-thiadiazole in 50 ml of tetrahydrofuran and after stirring at 20° C for 3 hours, 25 ml of isopropyl ether were added. The mixture was vacuum filtered and the recovered crystals were washed, dried and crystallized from acetone to obtain 5.2 g of 2-(N-methylcarbamoyl)-5-methylthio-1,2,4-thiadiazole-3-one melting at 144° C.

後処理

  1. filtrationfiltered
  2. washthe recovered crystals were washed
  3. customdried
  4. customcrystallized from acetone

出典と根拠

ORDレコード
ord-36dddd4f185c4c1b96818344c0dbb4ef
出典データセット
uspto-grants-1978_01
特許番号
US04067720

反応ノート

読み込み中…