HCID 59370741, compound → Hydrochloric Acid

HRID 1678720Notes

Reaction equation

HRID 1678720 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[CH2:10][O:9]2)=[CH:4][C:3]=1[NH:11][S:12]([CH3:15])(=[O:14])=[O:13].[CH:16]([C:19]1[C:27]2[C:22](=[CH:23][C:24]([O:28][CH2:29][CH2:30][NH2:31])=[CH:25][CH:26]=2)[NH:21][N:20]=1)([CH3:18])[CH3:17].CC(O)C.C(C1C2C(=CC(OCCN)=CC=2)NN=1)(C)C>CC(O)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]([OH:9])[CH2:10][NH:31][CH2:30][CH2:29][O:28][C:24]2[CH:23]=[C:22]3[C:27]([C:19]([CH:16]([CH3:18])[CH3:17])=[N:20][NH:21]3)=[CH:26][CH:25]=2)=[CH:4][C:3]=1[NH:11][S:12]([CH3:15])(=[O:14])=[O:13].[ClH:1]

Participants

6

Reactant 3

HCID 59370741HCID 59370741, compoundHCID 178440415HCID 178440415, compoundHCID 178459062HCID 178459062, compound

Product 2

HCID 313Hydrochloric AcidHCID 178440416HCID 178440416, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent2×

Procedure

2-Propanol (1.5 mL) was added to (R)-N-(2-chloro-5-(oxiran-2-yl)phenyl)methanesulfonamide (28.6 mg) that can be produced by the method described in Reference Example 69 or the like, and a 2-(3-isopropylindazol-6-yloxy)ethanamine-2-propanol solution [37.5 μL; solution prepared by dissolving 2-(3-isopropylindazol-6-yloxy)ethanamine (306.4 mg) that can be produced by the method described in Reference Example 68 or the like, in 2-propanol (347.5 μL)]. The mixture was stirred overnight at reflux. The reaction solution was cooled to room temperature, and then nitrogen gas was blown into the reaction solution to evaporate the solvent. The resulting residue was purified by HPLC, and then the purification product was dissolved in water (1 mL) and a 1 mol/L aqueous solution of hydrochloric acid (150 μL; manufactured by Kanto Chemical Co., Inc.). The solution was freeze-dried, and thus the title compound was obtained in the form of hydrochloride (18.1 mg).

Workup

  1. customcan be produced by the method
  2. customsolution prepared
  3. customcan be produced by the method
  4. temperatureat reflux
  5. customto evaporate the solvent
  6. customThe resulting residue was purified by HPLC
  7. dissolutionthe purification product was dissolved in water (1 mL)
  8. customThe solution was freeze-dried

Sources & evidence

ORD record
ord-38a1de5010384104b8d7a47e6e23314e
Source dataset
uspto-grants-2011_08
Patent number
US08008506B2

Reaction notes

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