Trifluoroacetic acid → HCID 88435369, compound

HRID 2259596Notes

Reaction equation

HRID 2259596 reaction equation
[CH2:1]([C:5]1[N:10]=[C:9]([Cl:11])[C:8]([CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:7]([CH2:18][C:19]2[CH:24]=[CH:23][C:22]([C:25]([O:27]C(C)(C)C)=[O:26])=[CH:21][CH:20]=2)[N:6]=1)[CH2:2][CH2:3][CH3:4].FC(F)(F)C(O)=O>C(Cl)Cl>[CH2:1]([C:5]1[N:10]=[C:9]([Cl:11])[C:8]([CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:7]([CH2:18][C:19]2[CH:20]=[CH:21][C:22]([C:25]([OH:27])=[O:26])=[CH:23][CH:24]=2)[N:6]=1)[CH2:2][CH2:3][CH3:4]

Participants

4

Reactant 2

HCID 6422Trifluoroacetic acidHCID 88434968HCID 88434968, compound

Product 1

HCID 88435369HCID 88435369, compoundYield 100.1%

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

160 mg of the product of Example 3 were introduced into 4 ml of methylene chloride and 1 ml of trifluoroacetic acid and after the mixture was stirred at ambient temperature for 2 hours 30 minutes, it was diluted with 20 ml of methylene chloride, washed twice with 10 ml of water, extracted again with 20 ml of methylene chloride and evaporated to dryness under reduced pressure to obtain 140 mg of product which was crystallized from 1 ml of methylene chloride with 3 ml of isopropyl ether added to it. After standing at rest for approximately 16 hours, separation took place to obtain 77 mg of the expected product melting at 130° C.

Workup

  1. washwashed twice with 10 ml of water
  2. extractionextracted again with 20 ml of methylene chloride
  3. customevaporated to dryness under reduced pressure

Sources & evidence

ORD record
ord-ed0a8e4539e842f7b020820ad86e40ae
Source dataset
uspto-grants-1995_12
Patent number
US05474996

Reaction notes

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