Phosphorus oxychloride → HCID 59755071, compound

HRID 556416Notes

Reaction equation

HRID 556416 reaction equation
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[CH:12]=[C:13]([CH3:28])[C:14]3[C:18]4[N:19]=[C:20]([CH2:24][CH2:25][CH3:26])[NH:21][C:22](=O)[C:17]=4[S:16][C:15]=3[N:27]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].O=P(Cl)(Cl)[Cl:31]>>[Cl:31][C:22]1[C:17]2[S:16][C:15]3[N:27]=[C:11]([C:5]4[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=4)[CH:12]=[C:13]([CH3:28])[C:14]=3[C:18]=2[N:19]=[C:20]([CH2:24][CH2:25][CH3:26])[N:21]=1

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 135453263HCID 135453263, compound

Product 1

HCID 59755071HCID 59755071, compoundYield 100.1%

Procedure

0.57 g (1.4 mmol) 7-(3,4-dimethoxyphenyl)-9-methyl-2-propyl-pyrido[3′,2′:4,5]thieno-[3,2-d]pyrimidin-4-one is refluxed in 8 ml (86.4 mmol) phosphoroxychloride for 9 h. Then, the product is poured onto about 50 g ice water. The precipitate is sucked off, washed with about 250 ml water, suck dried and dried in vacuo at 50° C. 0.58 g (96%) 4-chloro-7-(3,4-dimethoxyphenyl)-9-methyl-2-propyl-pyrido[3′,2′:4,5]-thieno[3,2-d]pyrimidine is obtained.

Workup

  1. washwashed with about 250 ml water, suck
  2. customdried
  3. customdried in vacuo at 50° C

Sources & evidence

ORD record
ord-2ff0e6ea14df4a5aabfef6e1f72b8340
Source dataset
uspto-grants-2011_11
Patent number
US08058285B2

Reaction notes

Loading…