Hydrochloric Acid → HCID 22363603, compound

HRID 962899Notes

Reaction equation

HRID 962899 reaction equation
[OH-].[Na+].[BH4-].[Na+].[ClH:5].[CH3:6][N:7]1[CH2:13][CH2:12][CH2:11][C:10](=[O:14])[CH2:9][CH2:8]1.Cl>O>[ClH:5].[CH3:6][N:7]1[CH2:13][CH2:12][CH2:11][CH:10]([OH:14])[CH2:9][CH2:8]1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 4311764Sodium borohydrideHCID 101978461-methylazepan-4-one Hydrochloride

Product 1

HCID 22363603HCID 22363603, compoundYield 90%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

100 ml of 1N sodium hydroxide solution is added to a solution of 18.9 g of sodium borohydride in 100 ml of water. A solution of 163.6 g of 1-methylperhydroazepin-4-one HCl in 100 ml of water is added dropwise at an internal temperature of 0° to 5° C. The mixture is stirred for 2 hours at 0° to 5° C. and then for 2 hours at room temperature. The pH is adjusted to 2 to 3 by addition of semi-concentrated hydrochloric acid. The mixture is evaporated to dryness in vacuo, the residue is taken up in 600 ml of isopropanol, the inorganic salts are separated off at 60° to 75° C. and the product is crystallised in an ice bath. The product is filtered and dried to constant weight in vacuo at elevated temperature. 149 g (90%) of 1-methylperhydroazepin-4-ol HCl is obtained.

Workup

  1. waitfor 2 hours at room temperature
  2. customThe mixture is evaporated to dryness in vacuo
  3. customthe inorganic salts are separated off at 60° to 75° C.
  4. customthe product is crystallised in an ice bath
  5. filtrationThe product is filtered
  6. customdried to constant weight in vacuo at elevated temperature

Sources & evidence

ORD record
ord-3868856ce5aa4c9082caec7a418e7028
Source dataset
uspto-grants-1998_06
Patent number
US05760221

Reaction notes

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