Hydrochloric Acid → HCID 22908200, compound

HRID 1379890Notes

Reaction equation

HRID 1379890 reaction equation
[CH3:1][C:2]1[C:11]([C:12]([NH:14][NH:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:13])=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][O:7]2.CC1C(C(N(C(C)(C)C)N)=O)=CC=C2C=1CCCO2.C(O)C.[ClH:42]>O>[ClH:42].[CH3:1][C:2]1[C:11]([C:12]([NH:14][NH:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:13])=[CH:10][CH:9]=[C:8]2[C:3]=1[CH2:4][CH2:5][CH2:6][O:7]2

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 10956364HCID 10956364, compoundHCID 22908199HCID 22908199, compound

Product 1

HCID 22908200HCID 22908200, compoundYield 68%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a solid consisting of 70% of 1-(5-methylchroman-6-carbonyl)-2-t-butyl hydrazine and 30% of 1-(5-methylchroman-6-carbonyl)-1-t-butyl hydrazine was added 10 ml of dehydrated ethanol containing 10% of hydrochloric acid and then the resultant was heated under reflux for 30 minutes. After cooling with ice and water, the precipitated crystals were filtered to obtain 0.88 g of 1-(5-methylchroman-6-carbonyl)-2-t-butyl hydrazine hydrochloride with a melting point of 217° to 220° C. in a yield of 68%. The filtrate was concentrated to obtain 0.25 g of ethyl methylchromanate with a melting point of 79° to 80° C. in a yield of 29%.

Workup

  1. temperaturethe resultant was heated
  2. temperatureunder reflux for 30 minutes
  3. filtrationthe precipitated crystals were filtered

Sources & evidence

ORD record
ord-d7d0f96af61d46eba815f57a5c324ea9
Source dataset
uspto-grants-1997_09
Patent number
US05672723

Reaction notes

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