HCID 178431913, compound → HCID 22139851, compound

HRID 1825912Notes

Reaction equation

HRID 1825912 reaction equation
ClC1SC=C(C)C=1NC([NH:10][CH:11]1[CH2:20][CH2:19][CH2:18][CH2:17][C:12]21[O:16][CH2:15][CH2:14][O:13]2)=N>Cl.O>[O:13]1[C:12]2([CH2:17][CH2:18][CH2:19][CH2:20][CH:11]2[NH2:10])[O:16][CH2:15][CH2:14]1

Participants

4

Reactant 1

HCID 178431913HCID 178431913, compound

Product 1

HCID 22139851HCID 22139851, compoundYield 192.3%

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-adc3c38c395642eb9bc0366601e51bb8
Source dataset
uspto-grants-2006_05
Patent number
US07049333B2

Reaction notes

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