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p-Toluenesulfonic acid → HCID 22591679, 화합물

HRID 22842
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HRID 22842 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[C:10]1[O:11][C:12]([C:15]23[CH2:22][CH2:21][C:18]([CH2:23][CH2:24][CH2:25][C:26]4([CH3:31])OCC[O:27]4)([CH2:19][CH2:20]2)[CH2:17][CH2:16]3)=[N:13][N:14]=1.C1(C)C=CC(S(O)(=O)=O)=CC=1>CC(C)=O>[Cl:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[C:10]1[O:11][C:12]([C:15]23[CH2:22][CH2:21][C:18]([CH2:23][CH2:24][CH2:25][C:26](=[O:27])[CH3:31])([CH2:19][CH2:20]2)[CH2:17][CH2:16]3)=[N:13][N:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

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HCID 6101p-Toluenesulfonic acidHCID 225916872-(2-Chloro-4-methoxyphenyl)-5-{4-[3-(2-methyl-1,3-dioxolan-2-yl)propyl]bicyclo[2.2.2]oct-1-yl}-1,3,4-oxadiazole

생성물 1

HCID 22591679HCID 22591679, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

2-(2-Chloro-4-methoxyphenyl)-5-{4-[3-(2-methyl-1,3-dioxolan-2-yl)propyl]bicyclo[2.2.2]oct-1-yl}-1,3,4-oxadiazole (5-G) (0.200 g) was stirred in a mixure of 90% acetone/10% water (20 mL). p-Toluenesulfonic acid (15 mg) was added to the solution. The reaction was heated to reflux for 1 h. The volume was reduced by evaporation of acetone in vacuo. The mixture was then layered with ethyl acetate (25 mL) and saturated sodium bicarbonate solution (25 mL). The ethyl acetate layer was extracted and dried (MgSO4). Solvent was removed in vacuo to afford pure 5-{4-[5-(2-chloro-4-methoxyphenyl)-1,3,4-oxadiazol-2-yl]bicyclo[2.2.2]oct-1-yl}pentan-2-one (5-H).

후처리

  1. temperatureThe reaction was heated
  2. temperatureto reflux for 1 h
  3. customThe volume was reduced by evaporation of acetone in vacuo
  4. extractionThe ethyl acetate layer was extracted
  5. dry with materialdried (MgSO4)
  6. customSolvent was removed in vacuo

출처 및 근거

ORD 기록
ord-d607f51bf884434cb388f56dfa39df2c
출처 데이터셋
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06849636B2

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