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Triethylamine → CarbaMic acid, N-[(1R)-1-[3-[6-(trifluoroMethyl)-1H-benziMidazol-2-yl]-5-isoxazolyl]ethyl]-, 1,1-diMethylethyl ester

HRID 2066912
Notes
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Reaction equation

HRID 2066912 reaction equation
[C:1]([O:5][C:6]([NH:8][C@@H:9]([C:11]1[O:15][N:14]=[C:13]([C:16](O)=O)[CH:12]=1)[CH3:10])=[O:7])([CH3:4])([CH3:3])[CH3:2].CCN(CC)CC.ClC(OCC(C)C)=O.[F:34][C:35]([F:45])([F:44])[C:36]1[CH:37]=[C:38]([NH2:43])[C:39]([NH2:42])=[CH:40][CH:41]=1>C1COCC1.O>[F:34][C:35]([F:44])([F:45])[C:36]1[CH:41]=[CH:40][C:39]2[N:42]=[C:16]([C:13]3[CH:12]=[C:11]([C@H:9]([NH:8][C:6](=[O:7])[O:5][C:1]([CH3:2])([CH3:3])[CH3:4])[CH3:10])[O:15][N:14]=3)[NH:43][C:38]=2[CH:37]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 4

HCID 8471TriethylamineHCID 62365Isobutyl chloroformateHCID 5208224-Trifluoromethyl-1,2-phenylenediamineHCID 57355520(R)-5-(1-(tert-butoxycarbonylamino)ethyl)isoxazole-3-carboxylic acid

Product 1

HCID 136088227CarbaMic acid, N-[(1R)-1-[3-[6-(trifluoroMethyl)-1H-benziMidazol-2-yl]-5-isoxazolyl]ethyl]-, 1,1-diMethylethyl ester
Yield 88.8%

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 8028TetrahydrofuranSolvent2×

Procedure

To a solution of (R)-5-(1-(tert-butoxycarbonylamino)ethyl)-isoxazole-3-carboxylic acid (55 g, 0.215 mol) and Et3N (36 mL, 0.26 mol) in THF (2 L) was added dropwise isobutyl chloroformate (33 mL, 0.26 mol) at −20° C. The reaction mixture was stirred for 1 hr, and a solution of 4-(trifluoromethyl)benzene-1,2-diamine (45.4 g, 0.26 mol) in THF was added. After stirring for 2 h at −20° C., the mixture was allowed to warm up to RT and stirred for another 2 hr. Water was added to quench the reaction and the reaction mixture was evaporated under reduced pressure to remove THF. The aqueous layer was extracted with ethyl acetate (2×). The combined organic layers were washed with water, dried over Na2SO4, filtered and concentrated. The residue was re-dissolved in acetic acid (250 mL) and stirred for 2 hr at 90° C. The solution was concentrated under vacuum and partitioned with ethyl acetate and water. The organic layer was separated, washed with water, Na2CO3 solution and brine, dried over Na2SO4, filtered and concentrated. The crude product was purified by column chromatography to afford compound N.7, (R)-tert-butyl 1-(3-(6-(trifluoromethyl)-1H-benzo[d]imidazol-2-yl)isoxazol-5-yl)ethylcarbamate (75.7 g, 88.8%). 1H NMR (DMSO-d6) δ 7.8 (m, 4H), 6.9 (s, 1H), 4.91 (m, 1H), 1.46 (d, 3H), 1.39 (s, 9H).

Workup

  1. stirringAfter stirring for 2 h at −20° C.
  2. stirringstirred for another 2 hr
  3. customto quench
  4. customthe reaction
  5. customthe reaction mixture was evaporated under reduced pressure
  6. customto remove THF
  7. extractionThe aqueous layer was extracted with ethyl acetate (2×)
  8. washThe combined organic layers were washed with water
  9. dry with materialdried over Na2SO4
  10. filtrationfiltered
  11. concentrationconcentrated
  12. dissolutionThe residue was re-dissolved in acetic acid (250 mL)
  13. stirringstirred for 2 hr at 90° C
  14. concentrationThe solution was concentrated under vacuum
  15. custompartitioned with ethyl acetate and water
  16. customThe organic layer was separated
  17. washwashed with water, Na2CO3 solution and brine
  18. dry with materialdried over Na2SO4
  19. filtrationfiltered
  20. concentrationconcentrated
  21. customThe crude product was purified by column chromatography

Sources & evidence

ORD record
ord-b5291a4ed8484bfeaa89b1cb7815a0b6
Source dataset
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08293752B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes