Sodium ethoxide → 2-(azetidin-1-yl)-1H-benzo[d]imidazole

HRID 1945975

반응식

HRID 1945975 반응식
[N:1]1([C:5]2[N:9](COCC[Si](C)(C)C)[C:8]3[CH:18]=[CH:19][CH:20]=[CH:21][C:7]=3[N:6]=2)[CH2:4][CH2:3][CH2:2]1.[O-]CC.[Na+]>CN(C=O)C.O>[N:1]1([C:5]2[NH:6][C:7]3[CH:21]=[CH:20][CH:19]=[CH:18][C:8]=3[N:9]=2)[CH2:4][CH2:3][CH2:2]1

참가 물질

5

반응물 2

HCID 2723922Sodium ethoxideHCID 596054842-(azetidin-1-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-benzo[d]imidazole

생성물 1

HCID 596058832-(azetidin-1-yl)-1H-benzo[d]imidazole수율 98.8%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
150 °C

실험 절차

Into a sealed vessel was placed crude 2-(azetidin-1-yl)-1-((2-(trimethylsilyl)ethoxy)methyl)-1H benzo[d]imidazole (0.55 g) and sodium ethoxide (1.2 g) in DMF (14 mL). The reacted was heated for 30 mins at 150° C. in an oil bath. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was dried with magnesium sulfate, filtered and concentrated to give 310 mg of 2-(azetidin-1-yl)-1H-benzo[d]imidazole as yellow solid.

후처리

  1. customInto a sealed vessel was placed
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layer was dried with magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-41b39422460e48fabb5008a97878fe71
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08394796B2

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