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1,4-Dioxa-8-azaspiro(4.5)decane → (3-Methyl-1,2,4-oxadiazol-5-yl)-4-piperidone ethylene ketal

HRID 1418375
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HRID 1418375 반응식
[CH3:1][C:2]1[N:6]=[C:5](C(Cl)(Cl)Cl)[O:4][N:3]=1.[CH2:11]1[O:20][C:14]2([CH2:19][CH2:18][NH:17][CH2:16][CH2:15]2)[O:13][CH2:12]1>C(O)C>[CH2:11]1[O:20][C:14]2([CH2:19][CH2:18][N:17]([C:5]3[O:4][N:3]=[C:2]([CH3:1])[N:6]=3)[CH2:16][CH2:15]2)[O:13][CH2:12]1
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참가 물질

4

반응물 2

HCID 674351,4-Dioxa-8-azaspiro(4.5)decaneHCID 709533-Methyl-5-(trichloromethyl)-1,2,4-oxadiazole

생성물 1

HCID 57153768(3-Methyl-1,2,4-oxadiazol-5-yl)-4-piperidone ethylene ketal수율 19.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3-Methyl-5-trichloromethyl-1,2,4-oxadiazole (Moussebois and Eloy, Helv. Chim. Acta 1964, 47, 838) (1 g, 5 mmol) and 4-piperidone ethylene ketal (1.5 g, 10 mmol) in ethanol (20 ml) were heated reflux overnight. The solvent was evaporated and the residue taken up in dichloromethane and filtered. The filtrate was washed with dilute HCl, dried over sodium sulphate and evaporated to leave a pale yellow oil (0.22 g). The acid washing was neutralised with solid sodium bicarbonate and extracted with dichloromethane. Evaporation gave further oil (0.17 g, total 0.39 g), MS (+EI) 225 (M+).

후처리

  1. temperaturereflux overnight
  2. customThe solvent was evaporated
  3. filtrationfiltered
  4. washThe filtrate was washed with dilute HCl
  5. dry with materialdried over sodium sulphate
  6. customevaporated

출처 및 근거

ORD 기록
ord-13487dec1f804d92a366f3492c25bde9
출처 데이터셋
uspto-grants-1999_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05883102

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