Phosphorus oxychloride → HCID 86677056, compound

HRID 70793

Reaction equation

HRID 70793 reaction equation
O=[C:2]1[N:10]2[C:6]([NH:7][C:8]3[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=32)=[C:5]([C:15]#[N:16])[C:4]2[CH2:17][CH2:18][S:19][CH2:20][C:3]1=2.P(Cl)(Cl)([Cl:23])=O>>[Cl:23][C:2]1[N:10]2[C:6](=[N:7][C:8]3[CH:14]=[CH:13][CH:12]=[CH:11][C:9]=32)[C:5]([C:15]#[N:16])=[C:4]2[CH2:17][CH2:18][S:19][CH2:20][C:3]=12

Participants

3

Reactant 2

HCID 24813Phosphorus oxychlorideHCID 7126864412-oxo-3,4,6,12-tetrahydro-1H-thiopyrano[4',3':4,5]pyrido[1,2-a]benzimidazole-5-carbonitrile

Product 1

HCID 86677056HCID 86677056, compound

Procedure

Phosphorus oxychloride (50 ml) was added to 12-oxo-3,4,6,12-tetrahydro-1H-thiopyrano[4′,3′:4,5]pyrido[1,2-a]benzimidazole-5-carbonitrile (16 g), followed by heating under reflux for 3 hours. The reaction liquid was concentrated under reduced pressure and the residue was poured into ice-water. The precipitate was collected by filtration and washed with water to obtain 12-chloro-3,4-dihydro-1H-thiopyrano[4′,3′:4,5]pyrido[1,2-a]benzimidazole-5-carbonitrile (18 g).

Workup

  1. temperatureby heating
  2. temperatureunder reflux for 3 hours
  3. customThe reaction liquid
  4. concentrationwas concentrated under reduced pressure
  5. additionthe residue was poured into ice-water
  6. filtrationThe precipitate was collected by filtration
  7. washwashed with water

Sources & evidence

ORD record
ord-4bf2ddefbab741d9a6d096f2b7885867
Source dataset
uspto-grants-2014_09
Patent number
US08822688B2

Linked notes

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