Triethylamine → 5-Trichloromethylthioamino-3-Trichloromethyl-1,2,4Thiadiazole

HRID 126973

反応式

HRID 126973 の反応式
[NH2:1][C:2]1[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=1.C(N(CC)CC)C.[Cl:18][C:19]([Cl:23])([Cl:22])[S:20]Cl>C1C=CC=CC=1>[Cl:18][C:19]([Cl:23])([Cl:22])[S:20][NH:1][C:2]1[S:6][N:5]=[C:4]([C:7]([Cl:10])([Cl:9])[Cl:8])[N:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 11666Trichloromethanesulfenyl chlorideHCID 6028483-(Trichloromethyl)-1,2,4-thiadiazol-5-amine

生成物 1

HCID 202887225-Trichloromethylthioamino-3-Trichloromethyl-1,2,4Thiadiazole収率 24%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a 3-neck flask equipped with condenser, thermometer, and stirring bar was added 11.7 g (0.05 mole) 5-amino-3trichloromethyl-1,2,4-thiadiazole, 5.1 g (0.05 mole) triethylamine and 150 milliliters of benzene. After 9.3 g (0.05 mole) trichloromethane-sulfenyl chloride was added, the reaction mixture was heated at reflux for 16 hours and filtered hot. The filtrate was evaporatd under vacuum to give an orange paste which was triturated with acetonitrile, filered and washed with petroleum ether to obtain 4.4 g (24% yield) of product; mp=180° C.

後処理

  1. customTo a 3-neck flask equipped with condenser
  2. temperaturethe reaction mixture was heated
  3. temperatureat reflux for 16 hours
  4. filtrationfiltered hot
  5. customto give an orange paste which
  6. customwas triturated with acetonitrile
  7. washwashed with petroleum ether

出典と根拠

ORDレコード
ord-dced1756a29340fbaeb70f1fe106d399
出典データセット
uspto-grants-1981_03
特許番号
US04254265

関連ノート

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