Triethylamine → HCID 20293156, compound

HRID 1413078Notes

Reaction equation

HRID 1413078 reaction equation
[CH2:1]([O:8][C:9]1[C:18]2[O:17][CH2:16][CH2:15][O:14][C:13]=2[C:12]([NH2:19])=[CH:11][CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl[C:28]([O:30][CH2:31][CH3:32])=[O:29]>C(Cl)(Cl)Cl>[CH2:1]([O:8][C:9]1[C:18]2[O:17][CH2:16][CH2:15][O:14][C:13]=2[C:12]([NH:19][C:28]([O:30][CH2:31][CH3:32])=[O:29])=[CH:11][CH:10]=1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 13020422HCID 13020422, compound

Product 1

HCID 20293156HCID 20293156, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

To a solution of 30 g of 5-benzyloxy-8-amino-1,4-benzodioxane (XX), code number 760 727, in 250 ml of chloroform, 21.3 ml of triethylamine, then slowly, at 0° C., 15.2 g of ethyl chloroformate were added. The solution was stirred for 7 hours, filtered and the filtrate was washed with a diluted hydrochloric acid solution, with water, with a solution of sodium bicarbonate and with water. The solvent was evaporated and the residue recrystallized in ethylacetate.

Workup

  1. filtrationfiltered
  2. washthe filtrate was washed with a diluted hydrochloric acid solution, with water, with a solution of sodium bicarbonate and with water
  3. customThe solvent was evaporated
  4. customthe residue recrystallized in ethylacetate

Sources & evidence

ORD record
ord-18b6a5f6187c43628fbaa7232a7a59b7
Source dataset
uspto-grants-1981_02
Patent number
US04248788

Reaction notes

Loading…