Potassium cyanate → HCID 18670178, compound

HRID 1059436Notes

Reaction equation

HRID 1059436 reaction equation
[NH2:1][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[S:11][C:10]3[N:12]=[CH:13][CH:14]=[N:15][C:9]=3[NH:8][C:7]=2[CH:16]=1.[O-:17][C:18]#[N:19].[K+]>C(O)(=O)C.O>[N:15]1[C:9]2[NH:8][C:7]3[CH:16]=[C:3]([CH2:2][NH:1][C:18]([NH2:19])=[O:17])[CH:4]=[CH:5][C:6]=3[S:11][C:10]=2[N:12]=[CH:13][CH:14]=1

Participants

5

Reactant 2

HCID 11378442Potassium cyanateHCID 18670209HCID 18670209, compound

Product 1

HCID 18670178HCID 18670178, compoundYield 14%

Reagents, catalysts & solvents 2

HCID 176Acetic AcidSolventHCID 962WaterSolvent2×

Procedure

A solution of 420 mg of 8-aminomethyl-10H-pyrazino[2,3-b][1,4]benzothiazine in acetic acid (2 ml)/water (4 ml) was heated to 70° C. and potassium cyanate (1 g in total) was added thereto over 2 hours. Then the reaction mixture was brought back to room temperature and diluted with water. The solid thus precipitated was filtered, washed well with water and recrystallized from dimethyl sulfoxide/ethyl acetate to thereby give 70 mg of the title compound as yellow crystals.

Workup

  1. customwas brought back to room temperature
  2. customThe solid thus precipitated
  3. filtrationwas filtered
  4. washwashed well with water
  5. customrecrystallized from dimethyl sulfoxide/ethyl acetate

Sources & evidence

ORD record
ord-150ce90ba53944c98580c9a7c6e1da1c
Source dataset
uspto-grants-2003_02
Patent number
US06518423B1

Reaction notes

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