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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2-(Dimethylamino)ethanol → 908117-05-5

HRID 912100
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HRID 912100 반응식
[H-].[Na+].[CH3:3][N:4]([CH3:8])[CH2:5][CH2:6][OH:7].[NH2:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12](Cl)[CH:11]=1>C1(C)C=CC=CC=1>[CH3:3][N:4]([CH3:8])[CH2:5][CH2:6][O:7][C:12]1[CH:11]=[C:10]([NH2:9])[CH:15]=[CH:14][N:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 79022-(Dimethylamino)ethanolHCID 24758Sodium hydrideHCID 844322-Chloropyridin-4-amine

생성물 1

HCID 59244595908117-05-5수율 62.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Sodium hydride (159 mg, 60% mineral oil dispersion, 3.98 mmol) was placed in a dried flask under a nitrogen atmosphere, followed by sequential addition of anhydrous toluene (10 ml) and 2-dimethylaminoethanol (177 mg, 2.0 mmol) with a syringe. After the resulting mixture was stirred at room temperature for 40 minutes, 4-amino-2-chloropyridine (203 mg, 1.59 mmol) was added, followed by heating to reflux for 16 hours. The reaction mixture was cooled, which was subsequently added dropwise slowly onto ice water, followed by extraction twice with ethyl acetate (10 ml). The organic layer was washed with brine (10 ml), and dried over sodium sulfate, followed by distilling off under reduced pressure, to obtain a crude product as a pale brown solid (180 mg).

후처리

  1. temperatureby heating
  2. temperatureto reflux for 16 hours
  3. temperatureThe reaction mixture was cooled
  4. additionwhich was subsequently added dropwise slowly onto ice water
  5. extractionfollowed by extraction twice with ethyl acetate (10 ml)
  6. washThe organic layer was washed with brine (10 ml)
  7. dry with materialdried over sodium sulfate
  8. distillationby distilling off under reduced pressure

출처 및 근거

ORD 기록
ord-257062406f7348df8796ea81175b7fe6
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022205B2

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