HCID 86753259, compound → HCID 86753256, compound

HRID 400074Notes

Reaction equation

HRID 400074 reaction equation
C(O)(=O)C(O)=O.[Cl:7][C:8]1[CH:9]=[C:10]([C@@:15]2([CH2:30][CH2:31][N:32]3[CH2:37][CH2:36][C:35]([C:41]4[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=4)([C:38]([NH2:40])=[O:39])[CH2:34][CH2:33]3)[CH2:19][CH2:18][N:17]([C:20](=[O:29])[C:21]3[CH:26]=[CH:25][C:24]([O:27][CH3:28])=[CH:23][CH:22]=3)[CH2:16]2)[CH:11]=[CH:12][C:13]=1[Cl:14]>ClCCl.CO>[Cl:7][C:8]1[CH:9]=[C:10]([C@@:15]2([CH2:30][CH2:31][N:32]3[CH2:37][CH2:36][C:35]([C:41]4[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=4)([C:38]([NH2:40])=[O:39])[CH2:34][CH2:33]3)[CH2:19][CH2:18][N:17]([C:20](=[O:29])[C:21]3[CH:22]=[CH:23][C:24]([O:27][CH3:28])=[CH:25][CH:26]=3)[CH2:16]2)[CH:11]=[CH:12][C:13]=1[Cl:14]

Participants

3

Reactant 1

HCID 86753259HCID 86753259, compound

Product 1

HCID 86753256HCID 86753256, compound

Reagents, catalysts & solvents 1

HCID 21226129Dichloromethane methanolSolvent

Procedure

Combine (R)-1-[2-[3-(3,4-dichloro-phenyl)-1-(4-methoxy-benzoyl)-pyrrolidin-3-yl]-ethyl]-4-phenyl-piperidine-4-carboxylic acid amide oxalic acid salt (6.5 g) and dichloromethane/methanol (300 mL/10 mL). Extract twice with a saturate aqueous solution of sodium bicarbonate, water and then brine. Dry the organic layer over MgSO4, filtered and evaporated in vacuo to give the title compound. Elemental Analysis calculated for C32H35 Cl2N3O3 : C 66.20; H 6.08; N 7.24; Found: C 65.92; H 6.06; N 7.03.

Workup

  1. extractionExtract twice with a saturate aqueous solution of sodium bicarbonate, water
  2. dry with materialDry the organic layer over MgSO4
  3. filtrationfiltered
  4. customevaporated in vacuo

Sources & evidence

ORD record
ord-c8c161488d144122871357599697ea7c
Source dataset
uspto-grants-1998_10
Patent number
US05824690

Reaction notes

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