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Chemical Structure| 1007882-59-8 Chemical Structure| 1007882-59-8

Structure of 1007882-59-8

Chemical Structure| 1007882-59-8

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Product Details of [ 1007882-59-8 ]

CAS No. :1007882-59-8
Formula : C12H18BrN3O2
M.W : 316.19
SMILES Code : O=C(N1[C@H](C2=NC=C(Br)N2)CCC1)OC(C)(C)C
MDL No. :MFCD16620748
InChI Key :GAZHEEFWONCMGH-QMMMGPOBSA-N
Pubchem ID :56605192

Safety of [ 1007882-59-8 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H302-H315-H319-H335
Precautionary Statements:P261-P305+P351+P338

Application In Synthesis of [ 1007882-59-8 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 1007882-59-8 ]

[ 1007882-59-8 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 1007882-59-8 ]
  • [ 1072946-50-9 ]
  • [ 1255936-29-8 ]
YieldReaction ConditionsOperation in experiment
To a solution of compound Int-lla (0.5 g, 1.58 mmol, prepared as described in U.S. Patent Publication No. US20090068140) in DME (15 mL) at room temperature under N2 was added PdCl2(dppf)2 (258 mg, 0.30 mmol). The reaction mixture was allowed to stir at 100 0C for 5 minutes, then a solution of compound Int-llb (592 mg, 3.16 mmol) and K2CO3 (654 mg, 4.74 mmol) in 15 mL H2O was added to the reaction mixture in 3 portions over 10 minutes. The resulting reaction was allowed to stir for an additional 30 minutes, after which time thin-layer chromatography analysis indicated consumption of compound Int-7a. The reaction was allowed to stir for an additional 30 minutes, then was concentrated in vacuo, and the residue obtained was taken up in 150 mL ethyl acetate. The organic phase was separated, washed with water (50 mL), brine and dried over sodium sulfate. After filtration, the organic layer was concentrated in vacuo and the resulting residue was purified using flash liquic chromatography (0% to 100% EtOAc/Hexane) to provide 600 mg of compound Int-llc (>; 85% purity, theory 597 mg). HPLC (C18 column Gemini 5u HOA, 150X21.2 mm, 5 micron). FABMS: MH+ = 379
To a solution of Compound Int-7d (0.5 g, 1.58 mmol) in DME (15 mL) at room temperature under N2 was added PdCl2(dppf)2 (258 mg, 0.30 mmol). The reaction mixture was allowed to stir at 100 0C for 5 minutes, then a solution of compound Int-19a (592 mg, 3.16 mmol) and K2CO3 (654 mg, 4.74 mmol) in 15 mL H2O was added to the reaction mixture in 3 portions over 10 minutes. The resulting reaction was allowed to stir for an additional 30 minutes, after which time thin-layer chromatography analysis indicated consumption of compound Int-7a. The reaction was allowed to stir for an additional 30 minutes, then was concentrated in vacuo, and the residue obtained was taken up in 150 niL ethyl acetate. The organic phase was separated, washed with water (50 rnL), brine and dried over sodium sulfate. After filtration, the organic layer was concentrated in vacuo and the resulting residue was purified using flash liquic chromatography (0% to 100% EtOAc/Hexane) to provide 600 mg of compound Int-19b (>; 85% purity, theory 597 mg). HPLC (C18 column Gemini 5u HOA, 150X21.2 mm, 5 micron). FABMS: MH+ = 379
  • 2
  • [ 1007882-59-8 ]
  • [ 1072946-50-9 ]
  • [ 1255936-29-8 ]
YieldReaction ConditionsOperation in experiment
EXAMPLE 15 Preparation of Intermediate Compound Int-15c (0321) (0322) To a solution of compound Int-7d (0.5 g, 1.58 mmol) in DME (15 mL) at room temperature under N2 was added PdCl2(dppf)2 (258 mg, 0.30 mmol). The reaction mixture was allowed to stir at 100 C for 5 minutes, then a solution of compound Int-15b (592 mg, 3.16 mmol) and K2CO3 (654 mg, 4.74 mmol) in 15 mL H2O was added to the reaction mixture in 3 portions over 10 minutes. The resulting reaction was allowed to stir for an additional 30 minutes, after which time thin-layer chromatography analysis indicated consumption of compound Int-7a. The reaction was allowed to stir for an additional 30 minutes, then was concentrated in vacuo, and the resulting residue was taken up in 150 mL ethyl acetate. The organic phase was separated, washed with water (50 mL), brine and dried over sodium sulfate. After filtration, the organic layer was concentrated in vacuo and the resulting residue was purified using flash liquid chromatography (0% to 100% EtOAc/Hexane) to provide 600 mg of compound Int-15c (> 85% purity, theory 597 mg). HPLC (C18 column Gemini 5u 110A, 150X21.2 mm, 5 micron). FABMS: MH+ = 379
 

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