HCID 178431913, compound → HCID 68456680, compound

HRID 2250502Notes

Reaction equation

HRID 2250502 reaction equation
[Cl:1][C:2]1[S:3][CH:4]=[C:5]([CH3:21])[C:6]=1[NH:7][C:8]([NH:10][CH:11]1[CH2:20][CH2:19][CH2:18][CH2:17][C:12]21OCCO2)=[NH:9]>Cl.O>[ClH:1].[Cl:1][C:2]1[S:3][CH:4]=[C:5]([CH3:21])[C:6]=1[N:7]1[C:12]2[CH2:17][CH2:18][CH2:19][CH2:20][C:11]=2[N:10]=[C:8]1[NH2:9]

Participants

4

Reactant 1

HCID 178431913HCID 178431913, compound

Product 1

HCID 68456680HCID 68456680, compoundYield 198.8%

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidSolvent2×HCID 962WaterSolvent

Procedure

N-(2-Chloro-4-methylthiophen-3-yl)-N′-(1,4-dioxaspiro[4.5]dec-6-yl)guanidine (24 mg) was dissolved in 2N hydrochloric acid (1 ml) and stirred at room temperature for 30 min. Concentrated hydrochloric acid (1 ml) was then added, and the mixture was stirred for another two hours. The mixture was then diluted with a little water and freeze-dried. Toluene was added to the residue and then distilled off under reduced pressure. This step was repeated twice, giving 22 mg of the desired product as a solid.

Workup

  1. stirringthe mixture was stirred for another two hours
  2. customfreeze-dried
  3. additionToluene was added to the residue
  4. distillationdistilled off under reduced pressure

Sources & evidence

ORD record
ord-5e7a6e7070354f9b91d1ee79f16c56df
Source dataset
uspto-grants-2008_01
Patent number
US07317033B2

Reaction notes

Loading…