Diethylamine → HCID 54736834, compound

HRID 1023680Notes

Reaction equation

HRID 1023680 reaction equation
[CH3:1][C:2]1[O:6][C:5]([C:7]([NH:9][C:10]([C:13]2[N:19]([CH3:20])[C:17](=[O:18])[C:16]([OH:21])=[C:15]([C:22]([NH:24][CH2:25][C:26]3[CH:27]=[CH:28][C:29]([F:32])=[CH:30][CH:31]=3)=[O:23])[N:14]=2)([CH3:12])[CH3:11])=[O:8])=[N:4][N:3]=1.[CH2:33]([NH:35][CH2:36][CH3:37])[CH3:34]>C(OCC)(=O)C>[CH3:1][C:2]1[O:6][C:5]([C:7]([NH:9][C:10]([C:13]2[N:19]([CH3:20])[C:17](=[O:18])[C:16]([OH:21])=[C:15]([C:22]([NH:24][CH2:25][C:26]3[CH:27]=[CH:28][C:29]([F:32])=[CH:30][CH:31]=3)=[O:23])[N:14]=2)([CH3:12])[CH3:11])=[O:8])=[N:4][N:3]=1.[CH2:33]([NH:35][CH2:36][CH3:37])[CH3:34]

Participants

4

Reactant 2

HCID 8021DiethylamineHCID 54671008Raltegravir

Product 1

HCID 54736834HCID 54736834, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

Raltegravir free hydroxy (24.6 mg) was suspended in ethyl acetate (0.250 mL) and diethylamine (6.4 μl) was added. The mixture was shaken well and the solid dissolved on heating. The resulting solution was temperature cycled between ambient and 50° C. using a Heidolph shaker and incubator with a power source programmed to switch on and off every 4 hours. After approximately 72 hours the solvent was allowed to evaporate under a flow of nitrogen and the solid residue was dried at ambient temperature under vacuum for approximately 24 hours. The product was characterised by XRPD.

Workup

  1. dissolutionthe solid dissolved
  2. temperatureon heating
  3. custom50° C.
  4. customoff every 4 hours
  5. customto evaporate under a flow of nitrogen
  6. customthe solid residue was dried at ambient temperature under vacuum for approximately 24 hours

Sources & evidence

ORD record
ord-de2383c7c7ab4e29991915e3e6d212d4
Source dataset
uspto-grants-2014_05
Patent number
US08722722B2

Reaction notes

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