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Sodium hydride → HCID 58504201, 화합물

HRID 2407694
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HRID 2407694 반응식
[H-].[Na+].[NH:3]1[CH2:8][CH2:7][CH:6]([CH2:9][OH:10])[CH2:5][CH2:4]1.Cl[C:12]1[C:17]2[C:18]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[N:19][O:20][C:16]=2[CH:15]=[N:14][N:13]=1>CN(C)C=O>[C:21]1([C:18]2[C:17]3[C:12]([O:10][CH2:9][CH:6]4[CH2:7][CH2:8][NH:3][CH2:4][CH2:5]4)=[N:13][N:14]=[CH:15][C:16]=3[O:20][N:19]=2)[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 4207714-PiperidinemethanolHCID 58504273HCID 58504273, 화합물

생성물 1

HCID 58504201HCID 58504201, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To sodium hydride (95% dispersion in mineral oil, 0.043 g) in N,N-dimethylformamide (6 mL) at 0° C. was added piperidin-4-ylmethanol (0.206 g). After stirring for 30 minutes, the compound prepared in Example 82 was added. The ice bath was removed and the reaction mixture was stirred at room temperature for two hours. The reaction mixture was then diluted with saturated a sodium bicarbonate solution and extracted with dichloromethane. The organics were dried over anhydrous magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (methanol:concentrated aqueous ammonia:dichloromethane=6:1:94) to obtain the title compound (0.20 g) having the following physical data.

후처리

  1. customThe ice bath was removed
  2. stirringthe reaction mixture was stirred at room temperature for two hours
  3. additionThe reaction mixture was then diluted with saturated a sodium bicarbonate solution
  4. extractionextracted with dichloromethane
  5. dry with materialThe organics were dried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography on silica gel (methanol:concentrated aqueous ammonia:dichloromethane=6:1:94)

출처 및 근거

ORD 기록
ord-857fe62b882f407986740d74c5fa7192
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809538B2

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