Diethylamine → HCID 15064526, compound

HRID 530262Notes

Reaction equation

HRID 530262 reaction equation
[NH:1]([CH2:4][CH3:5])[CH2:2][CH3:3].[Br:6][C:7]([F:14])([F:13])[C:8]([O:10]CC)=O>>[Br:6][C:7]([F:13])([F:14])[C:8]([N:1]([CH2:4][CH3:5])[CH2:2][CH3:3])=[O:10]

Participants

3

Reactant 2

HCID 8021DiethylamineHCID 69585Ethyl bromodifluoroacetate

Product 1

HCID 15064526HCID 15064526, compound

Procedure

Et2NH (7.9 g, 108 mmol) was added to ethyl bromodifluoroacetate (20.1 g, 99 mmol) at 30° C. The mixture was stirred for 60 min; then all volatiles were removed under reduced pressure. To the residue was added another 7.9 g of Et2NH and the mixture was stirred another 60 min. Again, all volatiles were removed under reduced pressure and the residue (16.3 g, >90% purity by NMR) was used in subsequent steps without further purification.

Workup

  1. customthen all volatiles were removed under reduced pressure
  2. additionTo the residue was added another 7.9 g of Et2NH
  3. stirringthe mixture was stirred another 60 min
  4. customAgain, all volatiles were removed under reduced pressure
  5. customthe residue (16.3 g, >90% purity by NMR) was used in subsequent steps without further purification

Sources & evidence

ORD record
ord-a4287d6e21b44250b5e38ebf01e22cee
Source dataset
uspto-grants-2016_05
Patent number
US09353070B2

Reaction notes

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