Trifluoroacetic acid → HCID 86656658, compound

HRID 882918Notes

Reaction equation

HRID 882918 reaction equation
C(O[C:6](=O)[N:7]([CH2:9][CH2:10][NH:11][C:12]([C:14]1[C:19]([NH2:20])=[N:18][C:17]([NH2:21])=[C:16]([Cl:22])[N:15]=1)=[O:13])C)(C)(C)C.[C:24]([OH:30])([C:26]([F:29])([F:28])[F:27])=[O:25].C(Cl)Cl.C(O)(C(F)(F)F)=O>C(Cl)Cl>[F:27][C:26]([F:29])([F:28])[C:24]([OH:30])=[O:25].[CH3:6][NH:7][CH2:9][CH2:10][NH:11][C:12]([C:14]1[C:19]([NH2:20])=[N:18][C:17]([NH2:21])=[C:16]([Cl:22])[N:15]=1)=[O:13]

Participants

5

Reactant 3

HCID 6422Trifluoroacetic acidHCID 21863450Trifluoroacetic acid methylene chlorideHCID 86656657HCID 86656657, compound

Product 1

HCID 86656658HCID 86656658, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A mixture comprising {2-[(3,5-diamino-6-chloro-pyrazine-2-carbonyl)-amino]-ethyl}-methyl-carbamic acid tert-butyl ester in DCM:TFA (60 mL of a 5:1 DCM/TFA solution) is stirred at RT for 3 h. The solvent is removed in vacuo and the resulting yellow oil is dissolved in water with heating. Any undissolved material is removed by filtration and the filtrate is concentrated in vacuo to afford the title compound. [M+H]+245.

Workup

  1. customThe solvent is removed in vacuo
  2. dissolutionthe resulting yellow oil is dissolved in water
  3. temperaturewith heating
  4. customAny undissolved material is removed by filtration
  5. concentrationthe filtrate is concentrated in vacuo

Sources & evidence

ORD record
ord-d05a7066205144e4bc61db80fb2c32cd
Source dataset
uspto-grants-2012_08
Patent number
US08236808B2

Reaction notes

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