Phosphorus oxychloride → HCID 21919323, compound

HRID 1244640Notes

Reaction equation

HRID 1244640 reaction equation
[OH:1][C:2]1[CH:19]=[CH:18][C:5]([CH2:6][C:7]2[N:11]3[N:12]=[C:13]([CH3:17])[C:14](O)=[N:15][C:10]3=[N:9][N:8]=2)=[CH:4][CH:3]=1.O=P(Cl)(Cl)[Cl:22]>>[Cl:22][C:14]1[C:13]([CH3:17])=[N:12][N:11]2[C:7]([CH2:6][C:5]3[CH:18]=[CH:19][C:2]([OH:1])=[CH:3][CH:4]=3)=[N:8][N:9]=[C:10]2[N:15]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 178433736HCID 178433736, compound

Product 1

HCID 21919323HCID 21919323, compound

Procedure

A solution of 3-(4-hydroxy-benzyl)-6-methyl-[1,2,4]triazolo[4,3-b][1,2,4]triazin-7-ol (170 mg, 0.62 mmol) in POCl3 (5 mL) was heated at 80° C. for 15 minutes, and then POCl3 was evaporated. The residue was purified on a silica gel column eluting with 5% methanol in dichloromethane to provide 4-(7-chloro-6-methyl-[1,2,4]triazolo[4,3-b][1,2,4]triazin-3-ylmethyl)-phenol (80 mg). MS (m/z) 275 [M+1].

Workup

  1. customPOCl3 was evaporated
  2. customThe residue was purified on a silica gel column
  3. washeluting with 5% methanol in dichloromethane

Sources & evidence

ORD record
ord-4d1d034a7ba140e09ad42b5b0060d859
Source dataset
uspto-grants-2006_10
Patent number
US07122548B2

Reaction notes

Loading…