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Potassium Carbonate → HCID 69423625, 화합물

HRID 1350124
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HRID 1350124 반응식
CC1(O)C(=[N:8][CH:9]([C:18]2[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=2)[CH2:10][CH2:11][CH:12]2[CH2:17][CH2:16][O:15][CH2:14][CH2:13]2)CC2CC1C2(C)C.Cl.NO.C([O-])([O-])=O.[K+].[K+]>C(O)C>[N:20]1[CH:21]=[CH:22][CH:23]=[C:18]([C@H:9]([NH2:8])[CH2:10][CH2:11][CH:12]2[CH2:13][CH2:14][O:15][CH2:16][CH2:17]2)[CH:19]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 21094262HCID 21094262, 화합물

생성물 1

HCID 69423625HCID 69423625, 화합물수율 80%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 2,6,6-trimethyl-3-(1-(3-pyridyl)-3-(4-oxanyl)propylimino]bicyclo[3.1.1]heptan-2-ol (1.85 g, 5.0 mmol) in ethanol (20 mL) was added hydroxylamine hydrochloride (2.00 g, 28.8 mmol) and K2CO3 (3.98 g, 28.8 mmol) and the mixture was heated to reflux for 16 h. The reaction was then cooled to room temperature, filtered through Celite, washed with ethanol, concentrated by rotary evaporation and purified by column chromatography, using a gradient of chloroform:methanol:ammonium hydroxide (90:9:1 to 80:19:1) eluent, to yield 0.88 g of a light yellow oil (80% yield).

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 16 h
  3. filtrationfiltered through Celite
  4. washwashed with ethanol
  5. concentrationconcentrated by rotary evaporation
  6. custompurified by column chromatography

출처 및 근거

ORD 기록
ord-4ccd22a9fea24132a94130b1a541323e
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07214686B2

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