Hydrochloric Acid → HCID 178479208, compound

HRID 904181Notes

Reaction equation

HRID 904181 reaction equation
[ClH:1].CO[C:4]1[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][N:5]=1.[NH2:11][NH:12][C:13]([NH:15][NH2:16])=[S:14]>CO>[ClH:1].[NH2:11][N:12]1[C:6]([CH2:7][CH2:8][CH2:9][CH2:10][CH2:4][NH2:5])=[N:16][N:15]=[C:13]1[SH:14]

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 756572H-Azepine, 3,4,5,6-tetrahydro-7-methoxy-HCID 2724189Thiocarbohydrazide

Product 1

HCID 178479208HCID 178479208, compoundYield 56.4%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To 200 ml of methanol is added 3.6 g (0.1 mole) of gaseous HCl followed by 12.7 g (0.1 mole) of O-methylcaprolactam and then 10.6 g (0.1 mole) of thiocarbohydrazide. After heating at reflux for 2 hours, the mixture is allowed to cool to room temperature and is refrigerated. The solid product is recrystallized twice from methanol/ethyl acetate, affording 13.4 g of 4-amino-5-(5-aminopentyl)-4H-1,2,4-triazole-3-thiol hydrochloride. m.p. 192°-194° C.

Workup

  1. temperatureAfter heating
  2. temperatureat reflux for 2 hours
  3. customThe solid product is recrystallized twice from methanol/ethyl acetate

Sources & evidence

ORD record
ord-1da6e09cca954a38909b63b99a891cdb
Source dataset
uspto-grants-1980_10
Patent number
US04230715

Reaction notes

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