Water → HCID 15295211, compound

HRID 725830Notes

Reaction equation

HRID 725830 reaction equation
[CH3:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].C(N(CC)CC)C.[Cl:16][C:17]1[N:18]=[C:19](Cl)[C:20]2[N:26]=[CH:25][N:24]=[C:23]([Cl:27])[C:21]=2[N:22]=1.O>C(Cl)Cl>[CH3:1][C:2]1[CH:3]=[C:4]([NH:5][C:19]2[C:20]3[N:26]=[CH:25][N:24]=[C:23]([Cl:27])[C:21]=3[N:22]=[C:17]([Cl:16])[N:18]=2)[CH:6]=[CH:7][CH:8]=1

Participants

6

Reactant 4

HCID 962WaterHCID 7934m-ToluidineHCID 8471TriethylamineHCID 2627202,4,8-trichloropyrimido[5,4-d]pyrimidine

Product 1

HCID 15295211HCID 15295211, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

0.45 g of 3-methylaniline and 0.42 g of triethylamine are added to 1.0 g of 2,4,8-trichloro-pyrimido[5,4-d]pyrimidine in 20 ml of methylene chloride at 0° to -10° C. and the mixture is stirred at this temperature for 1.5 hours. Water is then added and the organic phase is separated off, dried and concentrated. The residue is purified by chromatography over an aluminium oxide column with petroleum ether/ethyl acetate (10:2).

Workup

  1. customthe organic phase is separated off
  2. customdried
  3. concentrationconcentrated
  4. customThe residue is purified by chromatography over an aluminium oxide column with petroleum ether/ethyl acetate (10:2)

Sources & evidence

ORD record
ord-ecbf133a02de43d48247163a1c00b0f4
Source dataset
uspto-grants-1998_01
Patent number
US05707989

Reaction notes

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