Ether hydrochloride → HCID 66727447, compound

HRID 1845959Notes

Reaction equation

HRID 1845959 reaction equation
[CH3:1][C:2]1([CH3:22])[CH2:8][NH:7][CH2:6][CH2:5][CH2:4][N:3]1[S:9]([C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][CH:21]=1)[CH:18]=[N:17][CH:16]=[CH:15]2)(=[O:11])=[O:10].[ClH:23].C(OCC)C>ClCCl>[ClH:23].[ClH:23].[CH3:1][C:2]1([CH3:22])[CH2:8][NH:7][CH2:6][CH2:5][CH2:4][N:3]1[S:9]([C:12]1[CH:13]=[C:14]2[C:19](=[CH:20][CH:21]=1)[CH:18]=[N:17][CH:16]=[CH:15]2)(=[O:11])=[O:10]

Participants

4

Reactant 2

HCID 10953452Ether hydrochlorideHCID 49847789HCID 49847789, compound

Product 1

HCID 66727447HCID 66727447, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

64 mg of 6-(2,2-dimethyl-1,4-diazepan-1-ylsulfonyl)isoquinoline was dissolved in 5 mL of dichloromethane, and 1 mL of a 1 M hydrochloric acid-diethyl ether solution was added dropwise thereto with stirring and then reacted at room temperature for 3 hours. From the reaction solution, the solvent was distilled off, and the obtained residue was dissolved in 0.5 mL of methanol. Then, 5 mL of ethyl acetate was added with vigorous stirring, and the deposited yellow solid was dried to obtain 68 mg of the compound of interest as a yellow solid (87%).

Workup

  1. customreacted at room temperature for 3 hours
  2. distillationFrom the reaction solution, the solvent was distilled off
  3. dissolutionthe obtained residue was dissolved in 0.5 mL of methanol
  4. additionThen, 5 mL of ethyl acetate was added with vigorous stirring
  5. customthe deposited yellow solid was dried

Sources & evidence

ORD record
ord-009f5129ccc74990ab475d1ce8274e1b
Source dataset
uspto-grants-2015_02
Patent number
US08951997B2

Reaction notes

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