Dimethyl (aminoethyl)phosphonate

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of compound 6.2 (153 mg, 1 mmol) and the compound 1.7 (473 mg, 1 mmol) in DCE (5 mL) was added DIPEA (1.5 mmol) and HOAc (1.5 mmol). After stirring the mixture for 30 minutes, 2.0 mmol of NaBH(OAc)3 was added followed by Stirring the mixture overnight. 1.0 mL of 5M NaOH was added and the mixture was extracted with DCM (2×20 mL). Combined organics was washed with brine and dried over MgSO4. Filtration and concentration followed by purification through flash column chromatography on silica gel (10% methanol in DCM) to get pale brown powder. LCMS ESI(+) m/z: 612 (M+1). 1H NMR (CD3OD, 300 MHz) δ 8.64 (s, 1H), 8.45 (s, 1H), 8.13 (d, J=8.4 Hz, 1H), 7.89 (s, 1H), 7.73 (d, J=8.4 Hz, 1H), 7.61 (d, J=7.9 Hz, 1H), 7.38 (m, 1H), 7.28 (d, J=8.8 Hz, 1H), 7.23 (d, J=5.4 Hz, 1H), 7.05 (m, 1H), 6.90 (d, J=2.7 Hz, 1H), 6.44 (d, J=2.7 Hz, 1H), 5.20 (s, 2H), 3.73 (s, 3H), 3.70 (s, 3H), 2.90 (m, 2H), 2.10 (m, 2H). by Stirring the mixture overnight the mixture was extracted with DCM (2×20 mL) Combined organics was washed with brine dried over MgSO4 Filtration and concentration followed by purification through flash column chromatography on silica gel (10% methanol in DCM) to get pale brown powder

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of compound 6.2 (153 mg, 1 mmol) and the compound 1.7 (473 mg, 1 mmol) in DCE (5 mL) was added DIPEA (1.5 mmol) and HOAc (1.5 mmol). After stirring the mixture for 30 minutes, 2.0 mmol of NaBH(OAc)3 was added followed by Stirring the mixture overnight. 1.0 mL of 5M NaOH was added and the mixture was extracted with DCM (2×20 mL). Combined organics was washed with brine and dried over MgSO4. Filtration and concentration followed by purification through flash column chromatography on silica gel (10% methanol in DCM) to get pale brown powder. LCMS ESI(+) m/z: 612 (M+1). 1H NMR (CD3OD, 300 MHz) δ 8.64 (s, 1H), 8.45 (s, 1H), 8.13 (d, J=8.4 Hz, 1H), 7.89 (s, 1H), 7.73 (d, J=8.4 Hz, 1H), 7.61 (d, J=7.9 Hz, 1H), 7.38 (m, 1H), 7.28 (d, J=8.8 Hz, 1H), 7.23 (d, J=5.4 Hz, 1H), 7.05 (m, 1H), 6.90 (d, J=2.7 Hz, 1H), 6.44 (d, J=2.7 Hz, 1H), 5.20 (s, 2H), 3.73 (s, 3H), 3.70 (s, 3H), 2.90 (m, 2H), 2.10 (m, 2H). by Stirring the mixture overnight the mixture was extracted with DCM (2×20 mL) Combined organics was washed with brine dried over MgSO4 Filtration and concentration followed by purification through flash column chromatography on silica gel (10% methanol in DCM) to get pale brown powder

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of compound 6.2 (153 mg, 1 mmol) and the compound 1.7 (473 mg, 1 mmol) in DCE (5 mL) was added DIPEA (1.5 mmol) and HOAc (1.5 mmol). After stirring the mixture for 30 minutes, 2.0 mmol of NaBH(OAc)3 was added followed by Stirring the mixture overnight. 1.0 mL of 5M NaOH was added and the mixture was extracted with DCM (2×20 mL). Combined organics was washed with brine and dried over MgSO4. Filtration and concentration followed by purification through flash column chromatography on silica gel (10% methanol in DCM) to get pale brown powder. LCMS ESI(+) m/z: 612 (M+1). 1H NMR (CD3OD, 300 MHz) δ 8.64 (s, 1H), 8.45 (s, 1H), 8.13 (d, J=8.4 Hz, 1H), 7.89 (s, 1H), 7.73 (d, J=8.4 Hz, 1H), 7.61 (d, J=7.9 Hz, 1H), 7.38 (m, 1H), 7.28 (d, J=8.8 Hz, 1H), 7.23 (d, J=5.4 Hz, 1H), 7.05 (m, 1H), 6.90 (d, J=2.7 Hz, 1H), 6.44 (d, J=2.7 Hz, 1H), 5.20 (s, 2H), 3.73 (s, 3H), 3.70 (s, 3H), 2.90 (m, 2H), 2.10 (m, 2H). by Stirring the mixture overnight the mixture was extracted with DCM (2×20 mL) Combined organics was washed with brine dried over MgSO4 Filtration and concentration followed by purification through flash column chromatography on silica gel (10% methanol in DCM) to get pale brown powder