Methylamine → HCID 178485778, compound

HRID 2049563Notes

Reaction equation

HRID 2049563 reaction equation
[SH:1][C:2]1[N:6]([CH2:7][C:8]([O:10]CC)=O)[N:5]=[N:4][N:3]=1.[CH3:13][NH2:14]>C(O)C>[CH3:13][NH:14][C:8](=[O:10])[CH2:7][N:6]1[C:2]([SH:1])=[N:3][N:4]=[N:5]1

Participants

4

Reactant 2

HCID 6329MethylamineHCID 178472662HCID 178472662, compound

Product 1

HCID 178485778HCID 178485778, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Ethyl 5-mercapto-1H-tetrazol-1-ylacetate (2.0 g) was dissolved in 33% methylamine in ethanol (20 ml) and stood overnight at R.T. The solution was evaporated to dryness in vacuo, the residue dissolved in water (20 ml), adicified and ether extracted (6×50 ml). The extracts were dried and evaporated to give a crystalline solid which was crystallised from ethyl acetate, 0.59 g (32.0%) m.p. 167°-168°; δ[(CD3)2CO] 2.88 (3H,d, J 5 Hz, --NHCH3), 5.15 (2H,s, --CH2CO--), 6.70 (1H,m, --NH--), 12.9 (1H,bs, --SH). Found: C, 27.53; H, 4.17; N, 40.07; S, 18138. C4H7N5OS requires: C, 27.74; H, 4.07; N, 40.44; S, 18.51%.

Workup

  1. customThe solution was evaporated to dryness in vacuo
  2. dissolutionthe residue dissolved in water (20 ml)
  3. extractionether extracted (6×50 ml)
  4. customThe extracts were dried
  5. customevaporated
  6. customto give a crystalline solid which
  7. customwas crystallised from ethyl acetate, 0.59 g (32.0%) m.p. 167°-168°

Sources & evidence

ORD record
ord-27ff0ff53d62457e9cbe74433964d3e8
Source dataset
uspto-grants-1980_04
Patent number
US04198406

Reaction notes

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