Formic Acid → HCID 15580714, compound

HRID 543809Notes

Reaction equation

HRID 543809 reaction equation
C(O)=O.Cl[C:5]1[CH:6]=[C:7]([N:12]2[CH2:16][CH:15]([CH3:17])[C:14]([NH:18][CH:19]=[O:20])=[N:13]2)[CH:8]=[CH:9][C:10]=1[Cl:11]>O>[Cl:11][C:10]1[CH:5]=[CH:6][C:7]([N:12]2[CH2:16][CH:15]([CH3:17])[C:14]([NH:18][CH:19]=[O:20])=[N:13]2)=[CH:8][CH:9]=1

Participants

4

Reactant 2

HCID 284Formic AcidHCID 15580721HCID 15580721, compound

Product 1

HCID 15580714HCID 15580714, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

A 2.2 g. amount of the preceding compound is dissolved in 10.0 ml. of a mixture of formic acid and acetic anhydride (Example 15). The mixture is allowed to remain at room temperature for 3 hours. Water is added and a yellow solid is collected by filtration. The solid is dissolved in dichloromethane. The solution is dried over anhydrous magnesium sulfate and filtered through a hydrous magnesium silicate. The filtrate is concentrated while adding hexane until turbidity occurs. The mixture is cooled and filtered to give 2.1 g. of the product of the Example as a white solid, m.p. 172°-174° C.

Workup

  1. dissolutionamount of the preceding compound is dissolved in 10.0 ml
  2. filtrationa yellow solid is collected by filtration
  3. dissolutionThe solid is dissolved in dichloromethane
  4. dry with materialThe solution is dried over anhydrous magnesium sulfate
  5. filtrationfiltered through a hydrous magnesium silicate
  6. concentrationThe filtrate is concentrated
  7. additionwhile adding hexane until turbidity
  8. temperatureThe mixture is cooled
  9. filtrationfiltered
  10. customto give 2.1 g

Sources & evidence

ORD record
ord-3de2a625e169435c9e46c39fe2fb0873
Source dataset
uspto-grants-1984_05
Patent number
US04447442

Reaction notes

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