Methane → HCID 86737763, compound

HRID 1680009Notes

Reaction equation

HRID 1680009 reaction equation
[CH3:1][N:2]1[CH2:16][CH2:15][C:5]2([S:9]C=[N:7][CH:6]2[C:10]([O:12]CC)=[O:11])[CH2:4][CH2:3]1.C.[ClH:18]>>[ClH:18].[ClH:18].[NH2:7][CH:6]([C:5]1([SH:9])[CH2:4][CH2:3][N:2]([CH3:1])[CH2:16][CH2:15]1)[C:10]([OH:12])=[O:11]

Participants

4

Reactant 3

HCID 297MethaneHCID 313Hydrochloric AcidHCID 23458720HCID 23458720, compound

Product 1

HCID 86737763HCID 86737763, compoundYield 81%

Procedure

A solution of 113 g (0.466 mole) of ethyl 8-methyl-1-thia-3,8-diazaspiro-[4.5]dec-2-ene-4-carboxylate in 5 liters of approximately 6 N hydrochloric acid is heated under reflux for 4 hours. The solution is decolorized with activated charcoal and evaporated to dryness. Traces of water are eliminated by entrainment with benzene and isopropanol. The residue is then dissolved in 1.5 liter of ethanol, concentrated to a volume of approximately 400 ml and allowed to crystallize. In this way, 104.7 g of alpha-amino-4-mercapto-1-methyl-4-piperidine-acetic acid dihydrochloride is obtained; Yield: 81%; M.P. 201°-202° C. (decomposition).

Workup

  1. temperatureunder reflux for 4 hours
  2. customevaporated to dryness
  3. dissolutionThe residue is then dissolved in 1.5 liter of ethanol
  4. concentrationconcentrated to a volume of approximately 400 ml
  5. customto crystallize

Sources & evidence

ORD record
ord-6263b06493cf486085985005cd0c9637
Source dataset
uspto-grants-1981_06
Patent number
US04271172

Reaction notes

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