HCID 70378759, compound → HCID 13560839, compound

HRID 1194755Notes

Reaction equation

HRID 1194755 reaction equation
C(CCC=N[NH:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][S:15]([NH:18][CH3:19])(=[O:17])=[O:16])=[CH:10][CH:9]=1)#N>C(Cl)(Cl)Cl>[C:8]([CH2:9][C:10]1[C:9]2[C:8](=[CH:13][CH:12]=[C:11]([CH2:14][S:15]([NH:18][CH3:19])(=[O:16])=[O:17])[CH:10]=2)[NH:7][CH:11]=1)#[N:7]

Participants

3

Reactant 1

HCID 70378759HCID 70378759, compound

Product 1

HCID 13560839HCID 13560839, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

A suspension of the product from stage (a) (0.7 g) in polyphosphate ester (7 g) and chlorform (14 ml) was heated at reflux for 5 min. and then poured onto ice. The resulting suspension was stirred with ice for 20 min., then extracted with chloroform (4×20 ml) and the extract dried. Solvent was then removed and the residue purified by column chromatography (G). The title compound was obtained as a reddish semi-solid (0.38 g) which was impure and was employed directly in the next stage.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 5 min.
  3. additionpoured onto ice
  4. extractionextracted with chloroform (4×20 ml)
  5. customthe extract dried
  6. customSolvent was then removed
  7. customthe residue purified by column chromatography (G)

Sources & evidence

ORD record
ord-b83ea744aa8d48e681029812d0891c8e
Source dataset
uspto-grants-1989_03
Patent number
US04816470

Reaction notes

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