تفاعل #160071

معادلة التفاعل

tert-butyl 8-(2,2-difluoroethyl)-10-prop-2-ynoyl-11-oxa-3,8-diazaspiro[5.5]undecane-3-carboxylate

hydrazine

HCl

→

8-(2,2-difluoroethyl)-10-(1H-pyrazol-3-yl)-11-oxa-3,8-diazaspiro[5.5]undecane

المذيبات

ethanol

ethanol

ظروف التفاعل

المعالجة

1. 1
   تركيزThe solution was concentrated in vacuo
2. 2
   أخرىto give the crude pyrazole as a yellow oil
3. 3
   workup.ADDITIONwas added
4. 4
   تركيزThe reaction mixture was concentrated in vacuo

الإجراء التجريبي

A solution of tert-butyl 8-(2,2-difluoroethyl)-10-prop-2-ynoyl-11-oxa-3,8-diazaspiro[5.5]undecane-3-carboxylate (25 mg, 0.07 mmol), hydrazine (42 μL, 1.34 mmol) and ethanol (0.5 mL) was stirred for 1 hour at room temperature. The solution was concentrated in vacuo to give the crude pyrazole as a yellow oil. HCl (400 μL of 4 M in dioxane, 1.60 mmol) followed by ethanol (0.2 mL) was added and the reaction mixture was stirred for 15 minutes at room temperature. The reaction mixture was concentrated in vacuo to give 8-(2,2-difluoroethyl)-10-(1H-pyrazol-3-yl)-11-oxa-3,8-diazaspiro[5.5]undecane as a gummy yellow solid. ESI-MS m/z calc. 286.2. Found 287.1 (M+1)+; Retention time: 0.32 minutes (3 min run).

المصدر