Hydrogen chloride-ethyl acetate → HCID 66878502, compound

HRID 1015777Notes

Reaction equation

HRID 1015777 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-b56866fb3134498584c1fa8eca03de9d
Source dataset
uspto-grants-2011_07
Patent number
US07985862B2

Reaction notes

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