Diisopropylethylamine → HCID 178461598, compound

HRID 522802Notes

Reaction equation

HRID 522802 reaction equation
Cl[C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][NH:8]2)=[C:4]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][C@H:12]2[CH3:17])[N:3]=1.C(N(C(C)C)CC)(C)C.Cl.[CH3:28][C@@H:29]1[CH2:34][O:33][CH2:32][CH2:31][NH:30]1>CC(O)CC.C(Cl)Cl>[CH3:28][C@@H:29]1[CH2:34][O:33][CH2:32][CH2:31][N:30]1[C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][NH:8]2)=[C:4]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][C@H:12]2[CH3:17])[N:3]=1

Participants

6

Reactant 3

HCID 81531DiisopropylethylamineHCID 57356922(3R)-3-Methylmorpholine hydrochlorideHCID 178461592HCID 178461592, compound

Product 1

HCID 178461598HCID 178461598, compound

Reagents, catalysts & solvents 2

HCID 6344DichloromethaneSolventHCID 6568(+-)-2-ButanolSolvent

Conditions

Temperature
180 °C

Procedure

2-Chloro-6-((R)-3-methyl-morpholin-4-yl)-9H-purine (1.02 g, 4 mmol), diisopropylethylamine (1.40 mL, 8 mmol), and (R)-3-methylmorpholin hydrochloride (826 mg, 6 mmol) were stirred in 2-butanol (5 mL) in a closed microwave tube under argon at 50° C., until all ingredients were dissolved. The reaction was then stirred at 180° C. for 100 hours. The reaction mixture was then cooled to room temperature and diluted with 200 mL of CH2Cl2.

Workup

  1. dissolutionwere dissolved
  2. temperatureThe reaction mixture was then cooled to room temperature

Sources & evidence

ORD record
ord-b947f4e924834d29af0e3d3298ae2880
Source dataset
uspto-grants-2016_05
Patent number
US09334271B2

Reaction notes

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