Hydrochloric Acid → Ethyl benzo-1,2,3-thiadiazole-7-carboximidate hydrochloride

HRID 257138Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 257138
[C:1]([C:3]1[C:11]2[S:10][N:9]=[N:8][C:7]=2[CH:6]=[CH:5][CH:4]=1)#[N:2].[ClH:12].[CH2:13]([O:15]CC)[CH3:14]>C(O)C.O1CCCC1>[ClH:12].[S:10]1[C:11]2[C:3]([C:1](=[NH:2])[O:15][CH2:13][CH3:14])=[CH:4][CH:5]=[CH:6][C:7]=2[N:8]=[N:9]1

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 22182879Acibenzolar Acid Impurity 21

Produkt 1

HCID 20096457Ethyl benzo-1,2,3-thiadiazole-7-carboximidate hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

7.2 g of 7-cyanobenzo-1,2,3-thiadiazole are dissolved at 45° C. in 60 ml of absolute ethanol and 20 ml of tetrahydrofuran, and the solution is cooled to 0° C. and saturated with gaseous hydrochloric acid in the course of 1 hour at 0° C. to 15° C., with the exclusion of moisture. The reaction mixture is then stored for 24 hours in the refrigerator, treated with 70 ml of absolute diethyl ether and allowed to stand for another 4 days in the refrigerator. The solid is then filtered off, washed with diethyl ether and dried. This gives 9.4 g of compound 5.2 in the form of beige crystals of m.p. 270°-272° C.

Aufarbeitung

  1. waitto stand for another 4 days in the refrigerator
  2. filtrationThe solid is then filtered off
  3. washwashed with diethyl ether
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-6b8aba2cd88a4ef19a3d534e63efdd8e
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05260423

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