Water → Ethyl[3-(6-oxo-3-thiocarbamoyl-6h-pyridazin-1-yl-methyl)phenyl]carbamate

HRID 383644Notes

Reaction equation

[CH2:1]([O:3][C:4](=[O:22])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH2:12][N:13]2[C:18](=[O:19])[CH:17]=[CH:16][C:15]([C:20]#[N:21])=[N:14]2)[CH:7]=1)[CH3:2].[Cl-].C([NH2+]CC)C.O.[S-2:30].[Na+].[Na+].O>CN(C=O)C>[CH2:1]([O:3][C:4](=[O:22])[NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([CH2:12][N:13]2[C:18](=[O:19])[CH:17]=[CH:16][C:15]([C:20](=[S:30])[NH2:21])=[N:14]2)[CH:7]=1)[CH3:2]

Participants

Conditions

Temperature: 55 °C

Procedure

200 mg (0.67 mmol) of ethyl[3-(3-cyano-6-oxo-6H-pyridazin-1-ylmethyl)-phenyl]carbamate are dissolved in 1 ml of DMF, and 219 mg (2 mmol) of diethylammonium chloride and 165 mg (2 mmol) of sodium sulfide hydrate are added. The yellow suspension is stirred at 55° C. for 2 hours. 10 ml of water are added to the reaction mixture. The precipitate is filtered off with suction, washed with water and dried in vacuo. The substance is reacted further without further purification.

Workup

filtrationThe precipitate is filtered off with suction
washwashed with water
customdried in vacuo
customThe substance is reacted further without further purification

Sources & evidence

ORD record: ord-31010b8f76d946b3b04a246806827eee
Source dataset: uspto-grants-2013_02
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US08367668B2

Reaction notes

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