Dichloromethane → HCID 178472019, compound

HRID 1381999Notes

Reaction equation

HRID 1381999 reaction equation
C(O[CH:4]=[C:5]([C:11](=[O:22])[C:12]1[CH:17]=[C:16]([F:18])[C:15]([F:19])=[C:14]([F:20])[C:13]=1[F:21])[C:6]([O:8][CH2:9][CH3:10])=[O:7])C.C(Cl)Cl.Cl.[NH2:27][CH2:28][CH2:29][C:30]([O:32][CH2:33][CH3:34])=[O:31].C([O-])(O)=O.[Na+]>O>[CH2:33]([O:32][C:30]([CH2:29][CH2:28][NH:27][CH:4]=[C:5]([C:11](=[O:22])[C:12]1[CH:17]=[C:16]([F:18])[C:15]([F:19])=[C:14]([F:20])[C:13]=1[F:21])[C:6]([O:8][CH2:9][CH3:10])=[O:7])=[O:31])[CH3:34]

Participants

6

Reactant 4

HCID 6344DichloromethaneHCID 458475beta-Alanine, ethyl ester, hydrochlorideHCID 516892Sodium BicarbonateHCID 54346083Ethyl 3-ethoxy-2-(2,3,4,5-tetrafluorobenzoyl)acrylate

Product 1

HCID 178472019HCID 178472019, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

6.4 g of ethyl 3-ethoxy-2-(2,3,4,5-tetrafluoro-benzoyl)-acrylate are initially introduced into 30 ml of methylene chloride. A solution of 3.1 g of ethyl 3-amino-propionate hydrochloride in 12 ml of water is added to this. A solution of 1.7 g of NaHCO3 in 20 ml of water is added dropwise to the two-phase mixture with vigorous stirring. After the dropwise addition is complete, the mixture is stirred for a further 3 hours. The phases are then separated, and the organic phase is washed with water and dried over Na2SO4. After concentration, 7.8 g of the title compound remain.

Workup

  1. additionAfter the dropwise addition
  2. customThe phases are then separated
  3. washthe organic phase is washed with water
  4. dry with materialdried over Na2SO4
  5. concentrationAfter concentration, 7.8 g of the title compound

Sources & evidence

ORD record
ord-0a68c2cc5d7f4675a051ed9706e3b4c6
Source dataset
uspto-grants-1989_02
Patent number
US04804760

Reaction notes

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