Dichloromethane → HCID 86586598, compound

HRID 857720Notes

Reaction equation

HRID 857720 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].[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 86586598HCID 86586598, 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. is bubbled HCl (g) for 10 min. The flask is sealed and the reaction mixture is stirred at room temperature for 18 h. Nitrogen is bubbled through the reaction mixture for 5 min and the reaction mixture is concentrated to give C-(3-[1,2,4]Triazol-1-yl-pyridin-2-yl)-methylamine di hydrochloride as a white solid. 1H NMR (CD3OD, 400 MHz) δ 9.67 (s, 1H); 8.85 (d, J=5.3 Hz, 1 H); 8.72 (s, 1H); 8.18 (d, J=8 Hz, 1 H); 7.7 (dd, J=5.3, 8 Hz, 1 H); 4.45 (s, 2 H).

Workup

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

Sources & evidence

ORD record
ord-524ee4f05c764ad4ae0fe66e7ded34d3
Source dataset
uspto-grants-2006_12
Patent number
US07144899B2

Reaction notes

Loading…