Methyl Isocyanate → 1,3-Dimethyl-3-(5-benzylthio-1,3,4-thiadiazol-2-yl)urea

HRID 1391192ノート

反応式

HRID 1391192 の反応式
[CH3:1][NH:2][C:3]1[S:4][C:5]([S:8][CH2:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[N:6][N:7]=1.[CH3:16][N:17]=[C:18]=[O:19]>C(OCC)(=O)C>[CH3:16][NH:17][C:18]([N:2]([CH3:1])[C:3]1[S:4][C:5]([S:8][CH2:9][C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)=[N:6][N:7]=1)=[O:19]

参加物

4

反応物 2

HCID 12228Methyl IsocyanateHCID 8051175-(benzylthio)-N-methyl-1,3,4-thiadiazol-2-amine

生成物 1

HCID 233476281,3-Dimethyl-3-(5-benzylthio-1,3,4-thiadiazol-2-yl)urea

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 2-methylamino-5-benzylthio-1,3,4-thiadiazole (4.0 g) in ethyl acetate (100 ml) was added 1.5 g of methyl isocyanate. The reaction was stirred at room temperature for 2 hrs. then heated at reflux for an additional 2 hrs. The product, 1,3-dimethyl-3-(5-benzylthio-1,3,4-thiadiazol-2-yl)urea, crystallized upon the addition of petroleum ether, was collected, washed with ether and dried to give 4.7 g, MP 139°-142° C.

後処理

  1. temperaturethen heated
  2. temperatureat reflux for an additional 2 hrs
  3. customThe product, 1,3-dimethyl-3-(5-benzylthio-1,3,4-thiadiazol-2-yl)urea, crystallized upon the addition of petroleum ether
  4. customwas collected
  5. washwashed with ether
  6. customdried
  7. customto give 4.7 g, MP 139°-142° C.

出典と根拠

ORDレコード
ord-9f2c0ae4a1c94d62b5cc1ecf1e3d3ef3
出典データセット
uspto-grants-1979_02
特許番号
US04141717

反応ノート

読み込み中…