Hydrochloric Acid → HCID 21993629, compound

HRID 1978524Notes

Reaction equation

HRID 1978524 reaction equation
[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[C:8]([CH:34]=[CH:35][CH:36]=1)[O:9][CH2:10][CH2:11][CH2:12][N:13]1[CH2:18][CH2:17][CH:16]([NH:19][C:20]([C:22]2[S:32][C:31]3[N:33]4[C:24](=[CH:25][N:26]=[C:27]4[CH:28]=[CH:29][CH:30]=3)[CH:23]=2)=[O:21])[CH2:15][CH2:14]1)=[O:5])[CH3:2].[ClH:37]>C(O)C>[ClH:37].[ClH:37].[CH2:1]([O:3][C:4]([C:6]1[CH:7]=[C:8]([CH:34]=[CH:35][CH:36]=1)[O:9][CH2:10][CH2:11][CH2:12][N:13]1[CH2:18][CH2:17][CH:16]([NH:19][C:20]([C:22]2[S:32][C:31]3[N:33]4[C:24](=[CH:25][N:26]=[C:27]4[CH:28]=[CH:29][CH:30]=3)[CH:23]=2)=[O:21])[CH2:15][CH2:14]1)=[O:5])[CH3:2]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21993630HCID 21993630, compound

Product 1

HCID 21993629HCID 21993629, compoundYield 79%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a solution of 473.3 mg (0.93 mmol.) of N-[1-[3-(3-ethoxycarbonylphenoxy)propan-1-yl]piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (5 ml) was added, at room temperature, 2 ml (24 mmol.) of 12N hydrochloric acid. The mixture was stirred for several minutes. The reaction mixture was concentrated under reduced pressure. To the concentrate was added ethanol. The resulting crystals were collected by filtration and washed with ethanol and diethyl ether to give the object compound (425.4 mg, 79%) as orange crystals, m.p.140-145° C.

Workup

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionTo the concentrate was added ethanol
  3. filtrationThe resulting crystals were collected by filtration
  4. washwashed with ethanol and diethyl ether

Sources & evidence

ORD record
ord-82915cf716a240318507d07b12a0b878
Source dataset
uspto-grants-2001_05
Patent number
US06235731B1

Reaction notes

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