Hydrochloric Acid → HCID 15871738, compound

HRID 1738907Notes

Reaction equation

HRID 1738907 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH2:12][C:13]([CH3:19])([CH3:18])[CH2:14][N:15]([CH3:17])[CH3:16])[C:10](=[O:20])[C@@H:9]([CH2:21][C:22]([O:24]CC)=[O:23])[O:8][C@H:7]([C:27]3[C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=[CH:29][CH:28]=3)[C:6]=2[CH:37]=1.C(=O)([O-])[O-].[K+].[K+].Cl>CO.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH2:12][C:13]([CH3:18])([CH3:19])[CH2:14][N:15]([CH3:16])[CH3:17])[C:10](=[O:20])[C@@H:9]([CH2:21][C:22]([OH:24])=[O:23])[O:8][C@H:7]([C:27]3[C:36]4[C:31](=[CH:32][CH:33]=[CH:34][CH:35]=4)[CH:30]=[CH:29][CH:28]=3)[C:6]=2[CH:37]=1

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 15871737HCID 15871737, compound

Product 1

HCID 15871738HCID 15871738, compoundYield 76.9%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 962WaterSolvent

Procedure

Ethyl trans-7-chloro-5-(1-naphthyl)-1-(2,2-dimethyl-3-dimethylamino-propyl)-2- oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate (212 mg, 0.41 mmol) and potassium carbonate (112 mg, 0.83 mmol) were stirred in a mixture of MeOH (8 ml) and water (2.5 ml) for 18 hours at 60° C. The mixture was cooled to room temperature, acidified to pH 2 with 2N HCl and extracted several times with ethyl acetate. The combined organic layers were dried with MgSO4. The filtrate was concentrated under reduced pressure to give the title compound (156 mg, 76%).

Workup

  1. extractionextracted several times with ethyl acetate
  2. dry with materialThe combined organic layers were dried with MgSO4
  3. concentrationThe filtrate was concentrated under reduced pressure

Sources & evidence

ORD record
ord-b5daddc4e02b4af786a57d7e9073af19
Source dataset
uspto-grants-1999_10
Patent number
US05965553

Reaction notes

Loading…