Ethanol → HCID 20525133, compound

HRID 1702914Notes

Reaction equation

HRID 1702914 reaction equation
[CH2:1]1[C:3]2([CH2:8][NH:7][C:6](=[S:9])[NH:5][CH2:4]2)[CH2:2]1.C[I:11].[CH2:12](O)C>C(OCC)(=O)C>[IH:11].[CH3:12][S:9][C:6]1[NH:7][CH2:8][C:3]2([CH2:2][CH2:1]2)[CH2:4][N:5]=1

Participants

5

Reactant 3

HCID 702EthanolHCID 6328Methyl iodideHCID 13050833HCID 13050833, compound

Product 1

HCID 20525133HCID 20525133, compoundYield 93.5%

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Conditions

Temperature
45 °C

Procedure

A mixture of 5,7-diazaspiro[2.5]octane-6-thione (7.53 g; 0.053 mol), methyl iodide (8.43 g; 0.0594 mol) and absolute ethanol (26 ml) is stirred and heated at 45° C. for one hour until the reaction mixture becomes straw colored and homogeneous. Ethyl acetate is added with cooling, the precipitated crystalline material is collected and dried to afford 14.05 g (93.5% yield) of title product, m.p. 128°-130° C.

Workup

  1. temperaturewith cooling
  2. customthe precipitated crystalline material is collected
  3. customdried

Sources & evidence

ORD record
ord-66e6d2a3cfa24aef982cf0fa55a73820
Source dataset
uspto-grants-1982_09
Patent number
US04349553

Reaction notes

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