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

HRID 126973

반응식

HRID 126973 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-dced1756a29340fbaeb70f1fe106d399
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04254265

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