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Potassium Hydroxide → 3',4'-dihydro-2-oxospiro[piperidine-4,4'(1H)-quinoline]

HRID 266890
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반응식

HRID 266890 반응식
F[C:2](F)(F)[C:3]([NH2:5])=[O:4].[NH:8]1[CH2:13][CH2:12][C:11]2([C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)C(=O)C2)[CH2:10][CH2:9]1.[OH-].[K+]>CO.O>[O:4]=[C:3]1[CH2:2][C:11]2([C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[NH:8][CH2:9][CH2:10]2)[CH2:12][CH2:13][NH:5]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 18467060Spiro[1H-indene-1,4'-piperidin]-3(2H)-one trifluoroacetamide

생성물 1

HCID 677074473',4'-dihydro-2-oxospiro[piperidine-4,4'(1H)-quinoline]수율 91.1%

시약·촉매·용매 1

HCID 22242641Methanol--water (1/1)용매

실험 절차

A solution of 49 mg (0.157 mmol) of the high RF material from Step B in methanol/water 4:1 with excess potassium hydroxide was stirred over night. The solution was concentrated and water and ethyl acetate were added to the residue. The layers were separated and the aqueous layer was extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate and concentrated to give 31 mg (0.143 mmol) of the title compound.

후처리

  1. concentrationThe solution was concentrated
  2. additionwater and ethyl acetate were added to the residue
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with ethyl acetate
  5. dry with materialThe combined organic layers were dried over sodium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2bd4a4afe0854aea8e7bb6d120c912d0
출처 데이터셋
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05652235

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