Chloroform → HCID 67445136, compound

HRID 1666708

Reaction equation

HRID 1666708 reaction equation
Cl.[NH2:2][CH2:3][CH:4]([CH3:9])[C:5]([O:7][CH3:8])=[O:6].C(Cl)(Cl)Cl.Cl[C:15]1[O:16][C:17]2[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=2[N:19]=1>>[CH3:8][O:7][C:5](=[O:6])[CH:4]([CH3:9])[CH2:3][NH:2][C:15]1[O:16][C:17]2[CH:23]=[CH:22][CH:21]=[CH:20][C:18]=2[N:19]=1

Participants

4

Reactant 3

HCID 6212ChloroformHCID 119862-ChlorobenzoxazoleHCID 13063725Methyl 3-amino-2-methylpropanoate hydrochloride

Product 1

HCID 67445136HCID 67445136, compoundYield 70.4%

Conditions

Temperature
40 °C

Procedure

To the suspension of 0.55 g (4 mmol) methy 3-amino-2-methylpropionate hydrogen chloride salt and 4 ml chloroform 0.52 g (5.2 mmol) triethylamine and 0.3 g (2 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. 0.33 g title compound is obtained as white crystals. Mp: 89-90° 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-e6151e03b1cc4ccc8e0cef04df781c73
Source dataset
uspto-grants-2011_10
Patent number
US08044078B2

Linked notes

Loading…