2,2,2-Trifluoroethanol → 5-Cyclobutylaminomethyl-pyrazin-2-ylamine

반응식

[CH:1]1([NH:5][CH2:6][C:7]2[N:8]=[CH:9][C:10]([NH:13]C(=O)OC(C)(C)C)=[N:11][CH:12]=2)[CH2:4][CH2:3][CH2:2]1.FC(F)(F)CO>>[CH:1]1([NH:5][CH2:6][C:7]2[N:8]=[CH:9][C:10]([NH2:13])=[N:11][CH:12]=2)[CH2:2][CH2:3][CH2:4]1

참가 물질

반응물 2

HCID 64092,2,2-Trifluoroethanol

HCID 66742355Tert-butyl 5-((cyclobutylamino)methyl)pyrazin-2-ylcarbamate

생성물 1

HCID 667422585-Cyclobutylaminomethyl-pyrazin-2-ylamine수율 95%

반응 조건

온도: 150 °C

실험 절차

In a 15 mL microwave tube was dissolved tert-butyl 5-((cyclobutylamino)methyl)pyrazin-2-ylcarbamate (330 mg, 1.19 mmol, Eq: 1.00) in 2,2,2-trifluoroethanol (119 mg, 12 ml, 1.19 mmol, Eq: 1.00) and the resulting mixture was heated in seal tube at 150° C. for 3 hrs. The crude reaction mixture was concentrated in vacuo, treated with MeOH and re-concentrated to remove residual trifluoroethanol. The material was azeotroped with toluene to afford 200 mg (95%) of the title compound.

후처리

customThe crude reaction mixture
concentrationwas concentrated in vacuo
additiontreated with MeOH
concentrationre-concentrated
customto remove residual trifluoroethanol
customThe material was azeotroped with toluene

출처 및 근거

ORD 기록: ord-6299a31597ca4241ac6b41545b8a4b37
출처 데이터셋: uspto-grants-2013_07
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08481540B2

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