Methylamine → HCID 20266292, compound

HRID 1719670Notes

Reaction equation

HRID 1719670 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][CH2:9][CH:8]=[C:7](CCl)[C:6]=2[CH:13]=1.[CH3:14][NH2:15]>>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][CH2:9][CH:8]=[C:7]([NH:15][CH3:14])[C:6]=2[CH:13]=1

Participants

3

Reactant 2

HCID 6329MethylamineHCID 10822547HCID 10822547, compound

Product 1

HCID 20266292HCID 20266292, compound

Procedure

500 ml of 33% ethanolic methylamine are added dropwise with cooling by ice/water to 105 g of 6-chloro-4-chloromethyl-2H-1-benzopyrane. Reaction is continued for 8 hours at room temperature, the mixture concentrated by evaporation and the residue taken up in dichloromethane. This solution is washed with 500 ml each of 1N NaOH and water, dried over MgSO4 and concentrated by evaporation. Distillation of the residue yields the title product b.p.: 116-120/13.3 Pascal.

Workup

  1. customReaction
  2. concentrationthe mixture concentrated by evaporation
  3. washThis solution is washed with 500 ml each of 1N NaOH and water
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated by evaporation
  6. distillationDistillation of the residue

Sources & evidence

ORD record
ord-baab4b1640104d30936c244ec29d840d
Source dataset
uspto-grants-1985_09
Patent number
US04542022

Reaction notes

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