Ether hydrochloride → HCID 22481983, compound

HRID 2182160Notes

Reaction equation

HRID 2182160 reaction equation
C(OC(=O)[N:7]([CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=1)[C:8]1[N:13]=[C:12]([N:14]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[CH:11]=[N:10][CH:9]=1)(C)(C)C.[ClH:29].CCOCC>CO>[ClH:29].[F:27][C:23]1[CH:22]=[C:21]([CH:26]=[CH:25][CH:24]=1)[CH2:20][NH:7][C:8]1[N:13]=[C:12]([N:14]2[CH2:15][CH2:16][NH:17][CH2:18][CH2:19]2)[CH:11]=[N:10][CH:9]=1

Participants

4

Reactant 2

HCID 10953452Ether hydrochlorideHCID 69732631HCID 69732631, compound

Product 1

HCID 22481983HCID 22481983, compoundYield 81.6%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a solution of (3-fluoro-benzyl)-(3,4,5,6-tetrahydro-2H-[1,2′]bipyrazinyl-6′-yl)-carbamic acid tert-butyl ester I-4c (1.09 g, 2.82 mmol) in Methanol (6 mL) was treated with 1.0 M HCl/ether (28.2 mL, 28.2 mmol). The reaction mixture was stirred at ambient temperature for 19 h and concentrated in vacuo. The residue was repulped overnight in a mixture of Methanol (5 mL) and Ether (40 mL). The resulting tan solid was filtered and dried under high vacuum to afford the title compound 4-L (745 mg).

Workup

  1. concentrationconcentrated in vacuo
  2. additionThe residue was repulped overnight in a mixture of Methanol (5 mL) and Ether (40 mL)
  3. filtrationThe resulting tan solid was filtered
  4. customdried under high vacuum

Sources & evidence

ORD record
ord-083f232989d047a8a7c27b5c25822cb4
Source dataset
uspto-grants-2005_05
Patent number
US06894050B2

Reaction notes

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