Inhibitor of nedd8-activating enzyme
A technology of compounds, chemical entities, applied in the field of cell proliferation disorders, active compounds
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[0140] abbreviation
[0141] AcOH acetic acid
[0142] ACN acetonitrile
[0143] DABCO Triethylenediamine
[0144] DCM dichloromethane
[0145] DCP 4,6-Dichloropyrimidine
[0146] DEA diethylamine
[0147] DIPEA N,N-Diisopropylethylamine
[0148] DMSO Dimethyl Sulfoxide
[0149] Et 2 O diethyl ether
[0150] EtOAc ethyl acetate
[0151] EtOH ethanol
[0152] Et 3 N triethylamine
[0153] FA formic acid
[0154] h 2 O water
[0155] hours
[0157] IPAc isopropyl acetate
[0158] LC / MS liquid chromatography mass spectrometry
[0159] LDA lithium diisopropylamide
[0160] MTBE methyl tert-butyl ether
[0161] MeOH Methanol
[0162] min minutes
[0163] MS mass spectrometry
[0164] NMP N-methyl-2-pyrrolidone
[0165] rt room temperature
[0166] P 3 NO 4-Phenylpropylpyridine-N-oxide
[0167] TBS tert-butyldimethylsilyl
[0168] TFA trifluoroacetic acid
[0169] THF Tetrahydrofuran
[0170] TLC thin layer chromatograph...
example 1
[0177] Example 1. Synthesis of (1R,2S)-5-chloro-2-methoxyindan-1-amine (8)
[0178] Step 1: rel-(1aR,6aS)-4-Chloro-6,6a-dihydro-1aH-indeno[1,2-b]oxirane (2).
[0179]To a stirred solution of 4-phenylpropylpyridine-N-oxide (278 mg, 1.31 mmol) in dichloromethane (20 mL) at 0°C was added (R,R)-Jacobson's catalyst (237.0 mg, 0.3732mmol) and sodium hypochlorite solution (2.0M aqueous solution; 16mL, 32mmol). The resulting brown suspension was stirred at 0 °C for 15 minutes, then a solution of 6-chloro-1H-indene (1) (2.81 g, 18.6 mmol) in dichloromethane (20 mL) was added via syringe along with additional sodium hypochlorite (2.0 M in water; 16 mL, 32 mmol). The reaction was stirred at 0 °C for 1 hour, then the ice bath was removed and the reaction was stirred at room temperature for 1 hour. An aliquot was taken and TLC on silica gel (hexanes) showed that all starting material was consumed. The reaction was poured into brine and extracted with dichloromethane. The combined extr...
example 2
[0191] Example 2. Sulfamic acid {(1S,2S,4R)-4-[(6-{[(1R,2S)-5-chloro-2-methoxy-2,3-dihydro-1H-indene- Synthesis of 1-yl]amino}pyrimidin-4-yl)oxy]-2-hydroxycyclopentyl}methyl ester (I-216)
[0192] Step 1: rel-(1R,5R)-5-({[tert-butyl(dimethyl)silyl]oxy}methyl)cyclopent-2-en-1-ol (10).
[0193] rel-(1R,5R)-5-(hydroxymethyl)cyclopent-2-en-1-ol (47.20g, 0.4135mol), N,N-dimethylamino To a solution of pyridine (2.52 g, 0.0207 mol) and 1H-imidazole (30.97 g, 0.4549 mol) in dichloromethane (800 mL, 10 mol) was added tert-butyldimethylsilyl chloride (28.0 g, 0.186 mol). The reaction was stirred at 0 °C for 2.5 h at which time tert-butyldimethylsilyl chloride (28.0 g, 0.186 mol) was added. The reaction was stirred for another 2 hours. The reaction was quenched by adding saturated aqueous NaCl (200 mL) and water (200 mL). The layers were separated and the organic layer was washed with water (3×200 mL) and brine (1×200 mL), washed with Na 2 SO 4 Dry, filter and concentrate in vacuo. ...
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