Diethylamine → HCID 135670767, compound

HRID 1107333Notes

Reaction equation

HRID 1107333 reaction equation
CS([C:5]1[N:10]=[C:9]2[N:11]=[C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[O:22][CH2:23][CH2:24][CH3:25])[NH:13][C:14](=[O:15])[C:8]2=[CH:7][N:6]=1)(=O)=O.[CH2:26]([NH:28][CH2:29][CH3:30])[CH3:27]>ClCCl>[CH2:26]([N:28]([CH2:29][CH3:30])[C:5]1[N:10]=[C:9]2[N:11]=[C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[O:22][CH2:23][CH2:24][CH3:25])[NH:13][C:14](=[O:15])[C:8]2=[CH:7][N:6]=1)[CH3:27]

Participants

4

Reactant 2

HCID 8021DiethylamineHCID 1356707527-Methylsulphonyl-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine

Product 1

HCID 135670767HCID 135670767, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of 7-methylsulphonyl-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine (229 mg) and diethylamine (420 mg) in dichloromethane (8 ml) was stirred at ambient temperature for 3 hours. The reaction mixture was eluted from a silica column with diethyl ether:chloroform (4:1) and the combined fractions containing product were evaporated under reduced pressure to yield an oil which on trituration with 40-60° petroleum ether yielded the title compound, 85.5 mg, m.p. 116-7° C.

Workup

  1. washThe reaction mixture was eluted from a silica column with diethyl ether:chloroform (4:1)
  2. additionthe combined fractions containing product
  3. customwere evaporated under reduced pressure
  4. customto yield an oil which on trituration with 40-60° petroleum ether

Sources & evidence

ORD record
ord-e14af9efec9f476798cb1a24d4fa6aec
Source dataset
uspto-grants-2000_05
Patent number
US06060477

Reaction notes

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