HCID 22314541, compound → HCID 69725567, compound

HRID 966105Notes

Reaction equation

HRID 966105 reaction equation
[CH3:1][C:2]([NH:11][CH2:12][C:13]([C:15]1[CH:35]=[CH:34][C:18]2[O:19]C(C3C=CC=CC=3)(C3C=CC=CC=3)[O:21][C:17]=2[C:16]=1[O:36][CH3:37])=[O:14])([CH3:10])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1>Cl>[OH:21][C:17]1[C:16]([O:36][CH3:37])=[C:15]([C:13](=[O:14])[CH2:12][NH:11][C:2]([CH3:1])([CH3:10])[CH2:3][C:4]2[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=2)[CH:35]=[CH:34][C:18]=1[OH:19]

Participants

3

Reactant 1

HCID 22314541HCID 22314541, compound

Product 1

HCID 69725567HCID 69725567, compound

Reagents, catalysts & solvents 1

HCID 313Hydrochloric AcidSolvent2×

Procedure

34 g of the HCl salt of 2-(1,1-dimethyl-2-phenylethylamino)-1-(4-methoxy-2,2-diphenylbenzo[1,3]dioxol-5-yl)ethanone is refluxed in 340 mL of 15% methanolic hydrochloric acid for 2 hours. Then the solvent is distilled off under reduced pressure and the residue is dissolved in ethyl acetate. The solid precipitated is suction filtered and washed with ethyl acetate and diethyl ether. Yield: 18 g (77%, hydrochloride); melting point: 192° C.-196° C.

Workup

  1. distillationThen the solvent is distilled off under reduced pressure
  2. dissolutionthe residue is dissolved in ethyl acetate
  3. customThe solid precipitated
  4. filtrationfiltered
  5. washwashed with ethyl acetate and diethyl ether

Sources & evidence

ORD record
ord-9e9be5236d7448fa8420eea1fceeea77
Source dataset
uspto-grants-2005_10
Patent number
US06951888B2

Reaction notes

Loading…