Hydrochloric Acid → HCID 67073212, compound

HRID 1485366Notes

Reaction equation

HRID 1485366 reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.Cl.[CH2:9]([Cl:11])[Cl:10]>>[CH3:1][N:2]1[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.[CH2:9]([Cl:11])[Cl:10]

Participants

4

Procedure

To a solution of crude G or G′ (1 eq.) in anhydrous DCM were added at 0° C. H (1.3 eq.), followed by N-methylmorpholine (2.2 eq.) dropwise over 15 sec. The reaction mixture was stirred at rt for 10 minutes and, the milky suspension was poured into 1 M HCl. The aqueous phase was extracted with DCM. The organic phases were combined, washed with 1 M NaOH, brine, dried over MgSO4 and evaporated to dryness. The crude compound was purified by silica gel chromatography to afford the desired product (R)-I.

Workup

  1. extractionThe aqueous phase was extracted with DCM
  2. washwashed with 1 M NaOH, brine
  3. dry with materialdried over MgSO4
  4. customevaporated to dryness
  5. customThe crude compound was purified by silica gel chromatography

Sources & evidence

ORD record
ord-5ccbc00c836947128cd22da9b795031a
Source dataset
uspto-grants-2016_08
Patent number
US09422299B2

Reaction notes

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