Hydrogen chloride-ethyl acetate → HCID 66878502, compound

HRID 1015886Notes

Reaction equation

HRID 1015886 reaction equation
C(OC([NH:8][CH2:9][C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:11]=1[NH:17][C:18](=[O:21])[O:19][CH3:20])=O)(C)(C)C.C(OCC)(=O)C.Cl>C(O)C>[ClH:16].[NH2:8][CH2:9][C:10]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:11]=1[NH:17][C:18](=[O:21])[O:19][CH3:20]

Participants

4

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 86650831HCID 86650831, compound

Product 1

HCID 66878502HCID 66878502, compoundYield 170.5%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

(Step 3) To a solution (2 ml) of methyl (2-{[(t-butoxycarbonyl)amino]methyl}-4-chlorophenyl)carbamate obtained in Step 2 (1.25 g) in ethanol was added 4N hydrogen chloride-ethyl acetate solution (2 ml) at room temperature, and the mixture was stirred overnight. The resulting crystals were collected by filtration, and recrystallized from ethanol and ethyl acetate to give methyl [2-(aminomethyl)-4-chlorophenyl]carbamate hydrochloride (0.85 g) as a white solid.

Workup

  1. filtrationThe resulting crystals were collected by filtration
  2. customrecrystallized from ethanol and ethyl acetate

Sources & evidence

ORD record
ord-502aebe55f96489cbca87db1af370940
Source dataset
uspto-grants-2011_07
Patent number
US07985863B2

Reaction notes

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