HCID 15580721, compound → HCID 15580712, compound

HRID 543810Notes

Reaction equation

HRID 543810 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:13][CH:12]([CH3:14])[C:11]([NH:15][CH:16]=[O:17])=[N:10]2)[CH:5]=[CH:6][C:7]=1Cl>C(O)=O>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:13][CH:12]([CH3:14])[C:11]([NH:15][CH:16]=[O:17])=[N:10]2)[CH:5]=[CH:6][CH:7]=1

Participants

3

Reactant 1

HCID 15580721HCID 15580721, compound

Product 1

HCID 15580712HCID 15580712, compound

Reagents, catalysts & solvents 1

HCID 284Formic AcidSolvent

Procedure

A 3.0 g. amount of the preceding product is dissolved in 10 ml. of a mixture of formic acid and acetic anhydride (Example 15). The mixture is allowed to remain at room temperature for 3 hours, then is poured into ice water to separate a partial gum and solid. This material is collected, dissolved in dichloromethane and filtered through a short column of a hydrous magnesium silicate. The effluent is concentrated while adding hexane to separate 3.1 g. of the product of the Example as light yellow crystals, m.p. 140°-142° C.

Workup

  1. dissolutionamount of the preceding product is dissolved in 10 ml
  2. customto separate a partial gum and solid
  3. customThis material is collected
  4. dissolutiondissolved in dichloromethane
  5. filtrationfiltered through a short column of a hydrous magnesium silicate
  6. concentrationThe effluent is concentrated
  7. additionwhile adding hexane
  8. customto separate 3.1 g

Sources & evidence

ORD record
ord-a444070934bf446598dc71f275324cf8
Source dataset
uspto-grants-1984_05
Patent number
US04447442

Reaction notes

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