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[ CAS No. 2088458-39-1 ] {[proInfo.proName]}

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Product Details of [ 2088458-39-1 ]

CAS No. :2088458-39-1 MDL No. :MFCD31742743
Formula : C8H12N2O3 Boiling Point : -
Linear Structure Formula :- InChI Key :NJBGXPJITDKQPS-UHFFFAOYSA-N
M.W : 184.19 Pubchem ID :68457503
Synonyms :

Safety of [ 2088458-39-1 ]

Signal Word:Warning Class:
Precautionary Statements:P261-P280-P301+P312-P302+P352-P305+P351+P338 UN#:
Hazard Statements:H302-H315-H319-H335 Packing Group:
GHS Pictogram:

Application In Synthesis of [ 2088458-39-1 ]

* 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 [ 2088458-39-1 ]

[ 2088458-39-1 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 2088458-39-1 ]
  • [ 1895296-01-1 ]
  • [ 2229861-14-5 ]
YieldReaction ConditionsOperation in experiment
57% With di-isopropyl azodicarboxylate; triphenylphosphine In toluene at 110℃; for 16h; Large scale; A Step A: tert-Butyl 3-(3,3,3-trifluoro-2,2-dimethyl-propoxy)pyrazole-1- carboxylate A mixture of 3,3,3-trifluoro-2,2-dimethyl-propan-1-ol (10 g, 70.36 mmol) and tert-butyl 3-hydroxypyrazole-1-carboxylate (12.96 g, 70.36 mmol) in toluene (130 mL) was treated with triphenyl phosphine (20.30 g, 77.40 mmol) followed by isopropyl N-isopropoxycarbonyliminocarbamate (14.99 mL, 77.40 mmol) and the mixture was stirred at 110 °C for 16 hours. The yellow solution was concentrated under reduced pressure, diluted with heptane (100mL) and the precipitated triphenylphosphine oxide was removed by filtration and washed with heptane/toluene 4:1 (100mL). The yellow filtrate was evaporated and the residue purified by silica gel chromatography with a linear gradient of ethyl acetate in hexane (0-40%) to give tert-butyl 3-(3,3,3-trifluoro- 2,2-dimethyl-propoxy)pyrazole-1-carboxylate (12.3 g, 57%) as an off white solid. ESI- MS m/z calc.308.13477, found 309.0 (M+1)+; Retention time: 1.84 minutes.1H NMR (400 MHz, DMSO-d6) δ 8.10 (d, J = 3.0 Hz, 1H), 6.15 (d, J = 3.0 Hz, 1H), 4.18 (s, 2H), 1.55 (s, 9H), 1.21 (s, 6H).
57% With di-isopropyl azodicarboxylate; triphenylphosphine In toluene at 110℃; for 16h; 1.B.A Step A: tert-Butyl 3-(3,3,3-trifluoro-2,2-dimethyl-propoxy)pyrazole-l-carboxylate A mixture of 3,3,3-trifluoro-2,2-dimethyl-propan-l-ol (10 g, 70.36 mmol) and tert-butyl 3-hydroxypyrazole-l-carboxylate (12.96 g, 70.36 mmol) in toluene (130 mL) was treated with triphenyl phosphine (20.30 g, 77.40 mmol) followed by isopropyl N- isopropoxycarbonyliminocarbamate (14.99 mL, 77.40 mmol) and the mixture was stirred at 110 °C for 16 hours. The yellow solution was concentrated under reduced pressure, diluted with heptane (lOOmL) and the precipitated triphenylphosphine oxide was removed by filtration and washed with heptane/toluene 4: 1 (lOOmL). The yellow filtrate was evaporated and the residue purified by silica gel chromatography with a linear gradient of ethyl acetate in hexane (0-40%) to give tert-butyl 3-(3,3,3-trifluoro-2,2- dimethyl-propoxy)pyrazole-l-carboxylate (12.3 g, 57%) as an off white solid. ESI-MS m/z calc. 308.13477, found 309.0 (M+l) +; Retention time: 1.84 minutes. XH NMR (400 MHz, DMSO-d6) δ 8.10 (d, J = 3.0 Hz, 1H), 6.15 (d, = 3.0 Hz, 1H), 4.18 (s, 2H), 1.55 (s, 9H), 1.21 (s, 6H).
57% With di-isopropyl azodicarboxylate; triphenylphosphine In toluene at 110℃; for 16h; 1.B.A Step A: tert-Butyl 3-(3,3,3-trifluoro-2,2-dimethyl-propoxy)pyrazole-1-carboxylate A mixture of 3,3,3-trifluoro-2,2-dimethyl-propan-1-ol (10 g, 70.36 mmol) and tert-butyl 3-hydroxypyrazole-1-carboxylate (12.96 g, 70.36 mmol) in toluene (130 mL) was treated with triphenyl phosphine (20.30 g, 77.40 mmol) followed by isopropyl N-isopropoxycarbonyliminocarbamate (14.99 mL, 77.40 mmol) and the mixture was stirred at 110° C. for 16 hours. The yellow solution was concentrated under reduced pressure, diluted with heptane (100 mL) and the precipitated triphenylphosphine oxide was removed by filtration and washed with heptane/toluene 4:1 (100 mL). The yellow filtrate was evaporated and the residue purified by silica gel chromatography with a linear gradient of ethyl acetate in hexane (0-40%) to give tert-butyl 3-(3,3,3-trifluoro-2,2-dimethyl-propoxy)pyrazole-1-carboxylate (12.3 g, 57%) as an off white solid. ESI-MS m/z calc. 308.13477, found 309.0 (M+1)+; Retention time: 1.84 minutes. 1H NMR (400 MHz, DMSO-d6) δ 8.10 (d, J=3.0 Hz, 1H), 6.15 (d, J=3.0 Hz, 1H), 4.18 (s, 2H), 1.55 (s, 9H), 1.21 (s, 6H).
57% With di-isopropyl azodicarboxylate; triphenylphosphine In toluene at 110℃; for 16h; 1.C.2 Step 2: tert-Butyl 3-(3,3,3-trifluoro-2,2-dimethyl-propoxy)pyrazole-l- carboxylate A mixture of 3,3,3-trifluoro-2,2-dimethyl-propan-l-ol (10 g, 70.36 mmol) and tert-butyl 3-hydroxypyrazole-l-carboxylate (12.96 g, 70.36 mmol) in toluene (130 mL) was treated with triphenyl phosphine (20.30 g, 77.40 mmol) followed by isopropyl N- isopropoxycarbonyliminocarbamate (14.99 mL, 77.40 mmol) and the mixture was stirred at 110 °C for 16 hours. The yellow solution was concentrated under reduced pressure, diluted with heptane (lOOmL) and the precipitated triphenylphosphine oxide was removed by filtration and washed with heptane/toluene 4:1 (v:v) (lOOmL). The yellow filtrate was evaporated and the residue purified by silica gel chromatography with a linear gradient of ethyl acetate in hexane (0-40%) to give tert-butyl 3-(3,3,3-trifluoro- 2,2-dimethyl-propoxy)pyrazole-l-carboxylate (12.3 g, 57%) as an off white solid. ESI- MS m/z calc. 308.13477, found 309.0 (M+l)+; Retention time: 1.84 minutes. 1H NMR (400 MHz, DMSO-d6) d 8.10 (d, J = 3.0 Hz, 1H), 6.15 (d, J = 3.0 Hz, 1H), 4.18 (s, 2H), 1.55 (s, 9H), 1.21 (s, 6H).
57% With di-isopropyl azodicarboxylate; triphenylphosphine In toluene at 110℃; for 16h; C.2 Step 2: tert- Butyl 3-(3,3,3-trifluoro-2,2-dimethyl-propoxy)pyrazole-l- carboxylate A mixture of 3,3,3-trifluoro-2,2-dimethyl-propan-l-ol (10 g, 70.36 mmol) and tert- butyl 3-hydroxypyrazole-l-carboxylate (12.96 g, 70.36 mmol) in toluene (130 mL) was treated with triphenyl phosphine (20.30 g, 77.40 mmol) followed by isopropyl N- isopropoxycarbonyliminocarbamate (14.99 mL, 77.40 mmol) and the mixture was stirred at 110 °C for 16 hours. The yellow solution was concentrated under reduced pressure, diluted with heptane (lOOmL) and the precipitated triphenylphosphine oxide was removed by filtration and washed with heptane/toluene 4: 1 (v:v) (lOOmL). The yellow filtrate was evaporated and the residue purified by silica gel chromatography with a linear gradient of ethyl acetate in hexane (0-40%) to give /er/-butyl 3-(3,3,3-trifluoro- 2,2-dimethyl-propoxy)pyrazole-l-carboxylate (12.3 g, 57%) as an off white solid. ESI- MS m/z calc. 308.13477, found 309.0 (M+l) +; Retention time: 1.84 minutes. 1H NMR (400 MHz, DMSO-d6) d 8.10 ( d , J = 3.0 Hz, 1H), 6.15 (d, J= 3.0 Hz, 1H), 4.18 (s, 2H), 1.55 (s, 9H), 1.21 (s, 6H).
57% With di-isopropyl azodicarboxylate; triphenylphosphine In toluene at 110℃; for 16h; 1.A Step A: tert- Butyl 3-(3,3,3-trifluoro-2,2-dimethyl-propoxy)pyrazole-l-carboxylate A mixture of 3,3,3-trifluoro-2,2-dimethyl-propan-l-ol (10 g, 70.36 mmol) and tert- butyl 3-hydroxypyrazole-l-carboxylate (12.96 g, 70.36 mmol) in toluene (130 mL) was treated with triphenyl phosphine (20.30 g, 77.40 mmol) followed by isopropyl N-isopropoxycarbonyliminocarbamate (14.99 mL, 77.40 mmol) and the mixture was stirred at 110 °C for 16 hours. The yellow solution was concentrated under reduced pressure, diluted with heptane (lOOmL) and the precipitated triphenylphosphine oxide was removed by filtration and washed with heptane/toluene 4: 1 (lOOmL). The yellow filtrate was evaporated and the residue purified by silica gel chromatography with a linear gradient of ethyl acetate in hexane (0-40%) to give /er/-butyl 3-(3,3,3-trifluoro- 2,2-dimethyl-propoxy)pyrazole-l-carboxylate (12.3 g, 57%) as an off white solid. ESI- MS m/z calc. 308.13477, found 309.0 (M+l) +; Retention time: 1.84 minutes. NMR (400 MHz, DMSO-d6) d 8.10 (d, J = 3.0 Hz, 1H), 6.15 (d, J= 3.0 Hz, 1H), 4.18 (s, 2H), 1.55 (s, 9H), 1.21 (s, 6H).
57% With di-isopropyl azodicarboxylate; triphenylphosphine In toluene at 110℃; for 16h; 12.II.A Step A:
tert-Butyl 3-(3,3,3-trifluoro-2,2-dimethyl-propoxy)pyrazole-1-carboxylate (23) A mixture of 3,3,3-trifluoro-2,2-dimethyl-propan-1-ol (10 g, 70.36 mmol) and tert-butyl 3-hydroxypyrazole-1-carboxylate (12.96 g, 70.36 mmol) in toluene (130 mL) was treated with triphenyl phosphine (20.30 g, 77.40 mmol) followed by isopropyl N-isopropoxycarbonyliminocarbamate (14.99 mL, 77.40 mmol) and the mixture was stirred at 110° C. for 16 hours. The yellow solution was concentrated under reduced pressure, diluted with heptane (100 mL) and the precipitated triphenylphosphine oxide was removed by filtration and washed with heptane/toluene 4:1 (100 mL). The yellow filtrate was evaporated and the residue purified by silica gel chromatography with a linear gradient of ethyl acetate in hexane (0-40%) to give tert-butyl 3-(3,3,3-trifluoro-2,2-dimethyl-propoxy)pyrazole-1-carboxylate (12.3 g, 57%) as an off white solid. ESI-MS m/z calc. 308.13477, found 309.0 (M+1)+; Retention time: 1.84 minutes. 1H NMR (400 MHz, DMSO-d6) δ 8.10 (d, J=3.0 Hz, 1H), 6.15 (d, J=3.0 Hz, 1H), 4.18 (s, 2H), 1.55 (s, 9H), 1.21 (s, 6H).

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