Hydracrylonitrile → HCID 23004069, compound

HRID 382728Notes

Reaction equation

HRID 382728 reaction equation
[F:1][C:2]([F:15])([F:14])[CH2:3][O:4][CH2:5][C:6](=[O:13])[CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].OCC[C:19]#[N:20]>>[F:1][C:2]([F:14])([F:15])[CH2:3][O:4][CH2:5][C:6](=[O:13])[CH2:7][C:8]([O:10][CH2:11][CH2:12][C:19]#[N:20])=[O:9]

Participants

3

Reactant 2

HCID 8011HydracrylonitrileHCID 23004058HCID 23004058, compound

Product 1

HCID 23004069HCID 23004069, compoundYield 96%

Conditions

Temperature
142.5 °C

Procedure

A mixture of 4.04 g of ethyl 4-(2,2,2-trifluoroethyl)oxy-3-oxobutanoate (17.7 mmol) and 2.55 g of 3-hydroxypropionitrile (35.9 mmol) was heated at reflux temperature at a bath temperature of 135-150° C. at 10 torr for 6 hrs. The reflux condensor was replaced with a distillation head and the product was distilled under reduced pressure to give 4.26 g (96%) of the desired product as a viscous oil: bp 155-158° C. (1.5). The product was used in the next step after spectral characterization.

Workup

  1. temperaturewas heated
  2. distillationthe product was distilled under reduced pressure

Sources & evidence

ORD record
ord-04557b2af65d4d7aa3f4cbbcf83d5fcc
Source dataset
uspto-grants-2001_10
Patent number
US06310076B1

Reaction notes

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