Dimethylamine → HCID 131718267, compound

HRID 326807Notes

Reaction equation

HRID 326807 reaction equation
[Cl:1][C:2]1[C:11]2[C:6](=[C:7]([OH:13])[CH:8]=[CH:9][C:10]=2[Cl:12])[N:5]=[CH:4][N:3]=1.[CH3:14][NH:15][CH3:16].Cl.C(OCC)(=O)C>ClCCl>[ClH:1].[Cl:12][C:10]1[CH:9]=[CH:8][C:7]([OH:13])=[C:6]2[C:11]=1[C:2]([N:15]([CH3:16])[CH3:14])=[N:3][CH:4]=[N:5]2

Participants

5

Reactant 3

HCID 674Dimethylamine2×HCID 18952355HCID 18952355, compoundHCID 21866389Hydrogen chloride-ethyl acetate

Product 1

HCID 131718267HCID 131718267, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

A solution of 4,5-Dichloro-8-quinazolinol (0.6 g, 2.8 mmol) in dichloromethane is added to a saturated solution of dimethylamine gas in dichloromethane. The reaction mixture is stirred for 30 minutes, re-saturated with dimethylamine gas, stirred for 30 minutes and concentrated in vacuo to obtain a yellow solid. The solid is added to a 2.5% hydrochloric acid/ethyl acetate mixture. The mixture is filtered and the filter cake is washed with water and dried in a vacuum oven to give the title product as a white solid, 0.35 g, mp 232° C. (dec.).

Workup

  1. concentrationconcentrated in vacuo
  2. customto obtain a yellow solid
  3. filtrationThe mixture is filtered
  4. washthe filter cake is washed with water
  5. customdried in a vacuum oven

Sources & evidence

ORD record
ord-be9e2b76bfe14e8ea26f026620be1b51
Source dataset
uspto-grants-1993_12
Patent number
US05270466

Reaction notes

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