Girard’s reagent T Girard’s reagent T

Structural formula

• Numbering system
• Physical property data
• Toxicological data
• Ecological data
• Molecular structure data
• Computing chemical data
• More
  • Properties and Stability
  • Storage method
  • Synthesis method
  • Purpose

Numbering system

CAS number:123-46-6

MDL number:MFCD00012009

EINECS number:204-629-3

RTECS number:CP3150000

BRN number:3727163

PubChem number:24895356

Physical property data

1. Properties: White needle-like crystals. Strong hygroscopicity

2. Melting point: 188-192℃ (decomposition)

3. Solubility: easily soluble in water, soluble in 150 parts of absolute ethanol, soluble in ice Acetic acid, glycerin and ethylene glycol

Toxicological data

1. Acute toxicity: Rat oral LD: >500mg/kg

Ecological data

None yet

Molecular structure data

None yet

Compute chemical data

1. Reference value for hydrophobic parameter calculation (XlogP): None

2. Number of hydrogen bond donors: 2

3. Number of hydrogen bond acceptors: 3

4. Number of rotatable chemical bonds: 2

5. Number of tautomers: 2

6. Topological molecule polar surface area 55.1

7. Number of heavy atoms: 10

8. Surface charge: 0

9. Complexity: 105

10. Number of isotope atoms: 0

11. Determine the number of atomic stereocenters: 0

12. Uncertain number of atomic stereocenters: 0

13. Determine the number of chemical bond stereocenters: 0

14. Number of uncertain chemical bond stereocenters: 0

15. Number of covalent bond units: 2

Properties and stability

1. Properties: White needle-like crystals. Highly hygroscopic.

Storage method

None yet

Synthesis method

1. Preparation method: Mix ethyl chloroacetate and absolute ethanol, cool to 0°C, add trimethylamine pre-cooled to -5°C, control the exothermic reaction, and raise the reaction temperature to 60°C, after stopping the heat generation, place it at room temperature for 24 hours, add dropwise 100% hydrazine hydrate, stir for 45 minutes, cool, filter out the crystals, and dry to obtain Giralde’s reagent T, with a yield of 83.5%-89.5%.

2. Add 98.5 grams (84.5 liters, 0.8 mol) ethyl chloroacetate and 200 ml of absolute ethanol. Cool to 0°C, stop stirring, add 49 grams (74 ml, 0.83 mol) of trimethylamine pre-cooled to -5°C at one time, and use cooling to fully control the release.Carry out the reaction so that the temperature of the reactants rises to 60°C within about 10 working hours. After no longer exothermic, let the reactants stand at room temperature for 20 to 24 hours. Remove the condenser, replace the thermometer with a dropping funnel, add 40 grams (0.8 mol) of 100% hydrazine hydrate dropwise within 10-15 minutes under stirring, and continue stirring for 45 minutes. After the solution is slightly cooled, if the product does not crystallize automatically, rub the bottle wall with a glass rod to stimulate crystallization. The product will appear as fine colorless needle-shaped crystals. Cool in an ice bath, quickly filter out the easily deliquescent salt, wash with 1}} liters of absolute ethanol, press dry, and dry in a vacuum dryer filled with concentrated sulfuric acid. The product weighs 100 to 108 grams. After evaporating 200-300 ml of solvent from the mother liquor, a second batch of products was obtained, with a total weight of 112-120 grams (83.5-89.5%). The product should be stored in a dry, airtight container. After the product has been placed for a period of time,
it is best to recrystallize it with absolute ethanol before use.

Purpose

1. Used to separate estrone and 17-steroid compounds.

2.Separate ketones from mixtures containing non-ketone substances. Also used in some dehydration reactions.