Hydrochloric Acid → HCID 12279091, compound

HRID 1604984Notes

Reaction equation

HRID 1604984 reaction equation
[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[CH:6][C:7]2[O:11][N:10]=[C:9]([CH2:12][C:13](=[NH:17])OCC)[C:8]=2[CH:18]=1.[CH2:19](N)[CH2:20][NH2:21].Cl>C(O)C>[ClH:1].[NH:21]1[CH2:20][CH2:19][N:17]=[C:13]1[CH2:12][C:9]1[C:8]2[CH:18]=[C:4]([O:3][CH3:2])[CH:5]=[CH:6][C:7]=2[O:11][N:10]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3301EthylenediamineHCID 21548276HCID 21548276, compound

Product 1

HCID 12279091HCID 12279091, compoundYield 120.4%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

In ethanol (20 ml) was dissolved ethyl 5-methoxy-1,2-benzisoxazole-3-acetimidate hydrochloride (2.1 g) and thereto was added ethylenediamine (0.59 g) at room temperature. The mixture was stirred at room temperature for 3 hours and then kept in refrigerator overnight. To the mixture was added ethanol (10 ml) containing 20 % hydrochloric acid, and the precipitated crystallines were separated by filtration, washed with ether, dried and recrystallized from ethanol to give the desired compound (2.5 g). m.p. 240° to 252°C (decomp).

Workup

  1. customkept in refrigerator overnight
  2. customthe precipitated crystallines were separated by filtration
  3. washwashed with ether
  4. customdried
  5. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-598ebba9729f48f197bbabfa8edb19a8
Source dataset
uspto-grants-1976_04
Patent number
US03948928

Reaction notes

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