1,4-Dioxane hydrochloride → HCID 13890216, compound

HRID 2418519Notes

Reaction equation

HRID 2418519 reaction equation
[CH3:1][O:2][C:3](=[O:20])[C@@H:4]1[CH2:8][CH2:7][CH2:6][N:5]1[C:9](=[O:19])[CH2:10][NH:11]C(OC(C)(C)C)=O.O1CCOCC1.[ClH:27]>>[ClH:27].[CH3:1][O:2][C:3](=[O:20])[C@@H:4]1[CH2:8][CH2:7][CH2:6][N:5]1[C:9](=[O:19])[CH2:10][NH2:11]

Participants

3

Reactant 2

HCID 204431481,4-Dioxane hydrochlorideHCID 53986628HCID 53986628, compound

Product 1

HCID 13890216HCID 13890216, compoundYield 99%

Procedure

N-t-Butyloxycarbonyl-glycyl-L-proline methylester (21.3 g, 74.4 m mole) and 4N hydrogen chloride dioxan solution (150 ml) were mixed, and shaked to dissolve the solid material. It was stirred for 1 hour at room temperature. The solvent was well-distilled off under reduced pressure to obtain the solid glycyl-L-proline methylester hydrochloride (16.4 g, 73.9 m mole, yield: 99%). The product was very hygroscopic and gave a single spot with Rf =0.45 by silica gel thin layer chromatography (developing solvent, n-butanol:acetic acid:water=4:2:2, colour forming method: spraying of 0.1% ninhydrin and heating).

Workup

  1. dissolutionto dissolve the solid material
  2. distillationThe solvent was well-distilled off under reduced pressure

Sources & evidence

ORD record
ord-1b061f95bfde45bd95de335cd386aefc
Source dataset
uspto-grants-1984_09
Patent number
US04472381

Reaction notes

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