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

反応式

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

参加物

反応物 2

HCID 1118Sulfuric Acid2 回

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

生成物 1

HCID 126397022-(Trichloromethyl)-1,3,4-thiadiazole収率 92%

実験手順

At 180° to 190° C and over a period of 0.1 hour, a solution of 160.5 parts of 2,5-bis-trichloromethyl-1,3,4-thiadiazole in 200 parts by volume of concentrated H2SO4 is introduced into 100 parts by volume of concentrated H2SO4. The mixture is heated at 170° to 180° C for 0.15 hour, and then poured on to 2,000 parts of ice. The precipitated solid is suction filtered and washed with water. There is obtained 94 parts (92% of theory) of 2-trichloromethyl-1,3,4-thiadiazole; m.p.:57° C.

後処理

temperatureThe mixture is heated at 170° to 180° C for 0.15 hour
additionpoured on to 2,000 parts of ice
filtrationfiltered
washwashed with water

出典と根拠

ORDレコード: ord-19418c8fd78840f1a74654f2c78e884b
出典データセット: uspto-grants-1978_04
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04083986

反応ノート

読み込み中…

参加物