Chloroform → HCID 67445810, compound

HRID 1666707Notes

Reaction equation

HRID 1666707 reaction equation
Cl.[NH2:2][C@H:3]([C:5]([O:7][CH3:8])=[O:6])[CH3:4].C(Cl)(Cl)Cl.Cl[C:14]1[O:15][C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[N:18]=1>>[CH3:8][O:7][C:5](=[O:6])[C@H:3]([CH3:4])[NH:2][C:14]1[O:15][C:16]2[CH:22]=[CH:21][CH:20]=[CH:19][C:17]=2[N:18]=1

Participants

4

Reactant 3

HCID 6212ChloroformHCID 119862-ChlorobenzoxazoleHCID 2733257Alanine methyl ester hydrochloride

Product 1

HCID 67445810HCID 67445810, compoundYield 16.6%

Conditions

Temperature
40 °C

Procedure

To the suspension of 0.62 g (6 mmol) methyl alaninate hydrogen chloride salt and 4 ml chloroform 0.79 g (7.8 mmol) triethylamine and 0.46 g (3 mmol) 2-chloro-1,3-benzoxazole are added and the mixture is stirred at 40° C. for 4 hours and at room temperature for 12 hours. The chloroform solution is washed with water, citric acid solution and water, dried over sodium sulfate and evaporated in vacuum. The residue is treated with hexane, the crystals are filtered off and washed. 0.11 g title compound is obtained as white crystals. Mp: 112-113° C.

Workup

  1. additionare added
  2. washThe chloroform solution is washed with water, citric acid solution and water
  3. dry with materialdried over sodium sulfate
  4. customevaporated in vacuum
  5. additionThe residue is treated with hexane
  6. filtrationthe crystals are filtered off
  7. washwashed

Sources & evidence

ORD record
ord-b9d1d05f159b425a92a421769d56c57a
Source dataset
uspto-grants-2011_10
Patent number
US08044078B2

Reaction notes

Loading…