Sulfuric Acid → 2-(Trichloromethyl)-1,3,4-thiadiazole

반응식

[Cl:1][C:2]([Cl:13])([Cl:12])[C:3]1[S:4][C:5](C(Cl)(Cl)Cl)=[N:6][N:7]=1.S(=O)(=O)(O)O>>[Cl:1][C:2]([Cl:13])([Cl:12])[C:3]1[S:4][CH:5]=[N:6][N:7]=1

참가 물질

반응물 2

HCID 1118Sulfuric Acid

HCID 126396672,5-Bis(trichloromethyl)-1,3,4-thiadiazole

생성물 1

HCID 126397022-(Trichloromethyl)-1,3,4-thiadiazole수율 83%

실험 절차

6.4 parts by weight of 2,5-bis-trichloromethyl-1,3,4-thiadiazole is heated in 30 parts by volume of 91% sulfuric acid for 6 minutes at 175° to 185° C. The reaction mixture is subsequently poured carefully on to ice and the precipitated solid is filtered off. The reaction product is washed with water and treated with 20 parts by volume of methanol, and the minor amounts of undissolved starting material are filtered off. Concentration of the methanolic solution gives 3.4 parts (83% of theory) of 2-trichloromethyl-1,3,4-thiadiazole having a melting point of 58° C.

후처리

additionThe reaction mixture is subsequently poured carefully on to ice
filtrationthe precipitated solid is filtered off
washThe reaction product is washed with water
additiontreated with 20 parts by volume of methanol
filtrationare filtered off

출처 및 근거

ORD 기록: ord-797aee6e2b724ad3b0b420e404547833
출처 데이터셋: uspto-grants-1978_01
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US04066775

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