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Ammonia → 3-Azabicyclo[3.2.1]octan-6-one ethylene ketal

HRID 749119
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인쇄 미리보기

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HRID 749119 반응식
CS(O[CH2:6][CH:7]1[CH2:15][CH:14]([CH2:16]OS(C)(=O)=O)[CH2:13][C:8]21[O:12][CH2:11][CH2:10][O:9]2)(=O)=O.[NH3:22]>>[CH2:11]1[O:12][C:8]2([CH2:13][CH:14]3[CH2:15][CH:7]2[CH2:6][NH:22][CH2:16]3)[O:9][CH2:10]1
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참가 물질

3

반응물 2

HCID 222AmmoniaHCID 574863466,8-Bis(methylsulfonyloxymethyl)-1,4-dioxaspiro[4.4]nonane

생성물 1

HCID 597519893-Azabicyclo[3.2.1]octan-6-one ethylene ketal수율 100%

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온도
60 °C

실험 절차

6,8-Bis(methanesulfonyloxymethyl)-1,4-dioxaspiro[4.4]nonane (14.90 g, 43.3 mmol) was suspended in aqueous ammonia (35%, 150 ml) and heated for 18 h at 60° C. The reaction was cooled to ambient temperature and concentrated by rotary evaporation. The residue was treated with saturated sodium chloride solution (50 ml) and extracted with chloroform (3×50 ml). The organic extracts were combined, dried over sodium sulfate, filtered and concentrated to yield a brown oil (7.69 g, 100%).

후처리

  1. temperatureThe reaction was cooled to ambient temperature
  2. concentrationconcentrated by rotary evaporation
  3. additionThe residue was treated with saturated sodium chloride solution (50 ml)
  4. extractionextracted with chloroform (3×50 ml)
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-6286ecdb430c43e988a53e82262d39d5
출처 데이터셋
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07402592B2

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