MAGNESIUM SILICATE (synthetic) → HCID 14390461, compound

HRID 2072949Notes

Reaction equation

HRID 2072949 reaction equation
[CH2:1]([O:3][C:4](=[O:22])[CH2:5][NH:6][C:7]1[C:12]([NH:13][C:14](=O)[C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[CH:11][CH:10]=[CH:9][N:8]=1)[CH3:2].[O-][Si]([O-])=O.[Mg+2]>C(Cl)Cl>[CH2:1]([O:3][C:4](=[O:22])[CH2:5][N:6]1[C:7]2=[N:8][CH:9]=[CH:10][CH:11]=[C:12]2[N:13]=[C:14]1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH3:2]

Participants

4

Reactant 2

HCID 61680MAGNESIUM SILICATE (synthetic)HCID 14390484HCID 14390484, compound

Product 1

HCID 14390461HCID 14390461, compoundYield 39%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

N-[3-(benzoylamino)-2-pyridinyl]glycine ethyl ester, 10.32 g (0.034 mole) in two divided portions was heated in glass in a Wood's metal bath at 190° C. under a flow of nitrogen, one portion for 15 min and the other for 7 min. The green glassy residues were dissolved in methylene chloride, combined, and stirred together with 90 g of Florisil® for 1 hr. The mixture was filtered, and the filtrate evaporated to an oil, which crystallized. The solid was recrystallized from hexanes to give a crystalline solid, which was dried under high vacuum at room temperature overnight to give 3.67 g (39%) of crystals, m.p. 93°-95° C.

Workup

  1. filtrationThe mixture was filtered
  2. customthe filtrate evaporated to an oil, which
  3. customcrystallized
  4. customThe solid was recrystallized from hexanes
  5. customto give a crystalline solid, which
  6. customwas dried under high vacuum at room temperature overnight

Sources & evidence

ORD record
ord-cfa01b2a84684161aaf5556703c7cd46
Source dataset
uspto-grants-1990_04
Patent number
US04914109

Reaction notes

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