Dichloromethane → HCID 22185123, compound

HRID 1795269Notes

Reaction equation

HRID 1795269 reaction equation
C(OC(=O)[NH:7][CH2:8][C:9]1[C:14]([N:15]2[CH:19]=[N:18][CH:17]=[N:16]2)=[CH:13][CH:12]=[CH:11][N:10]=1)(C)(C)C.C(Cl)[Cl:22]>CO>[ClH:22].[N:15]1([C:14]2[C:9]([CH2:8][NH2:7])=[N:10][CH:11]=[CH:12][CH:13]=2)[CH:19]=[N:18][CH:17]=[N:16]1

Participants

4

Reactant 2

HCID 6344DichloromethaneHCID 69590386HCID 69590386, compound

Product 1

HCID 22185123HCID 22185123, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

Through a solution of (3-[1,2,4]triazol-1-yl-pyridin-2-ylmethyl)-carbamic acid tert-butyl ester (4.08 g) in CH2Cl2 (100 ml) and MeOH (20 ml) cooled to 0° C. was bubbled HCl (g) for 10 min. The flask was sealed and the reaction mixture was stirred at room temperature for 18 h. Nitrogen was bubbled through the reaction mixture for 5 min and the reaction mixture was concentrated to give C-(3[1,2,4]triazol-1-yl-pyridin-2-yl)-methylamine hydrochloride salt as a white solid. 1H NMR (CD3OD, 400 MHz) δ 9.67 (s, 1H); 8.85 (d, J=5.3 Hz, 1H); 8.72 (s, 1H); 8.18 (d, J=8 Hz, 1H); 7.7 (dd, J=5.3, 8 Hz, 1H); 4.45 (s, 2H).

Workup

  1. customwas bubbled HCl (g) for 10 min
  2. customThe flask was sealed
  3. customNitrogen was bubbled through the reaction mixture for 5 min
  4. concentrationthe reaction mixture was concentrated

Sources & evidence

ORD record
ord-be69cb4844cc46ada7ec8d795bd09093
Source dataset
uspto-grants-2006_04
Patent number
US07026324B2

Reaction notes

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