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4-Fluorobenzylamine → HCID 178522995, 화합물

HRID 2267101
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HRID 2267101 반응식
CO[C:3](=[O:21])[C:4]1[C:9]([OH:10])=[C:8]([O:11][CH2:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:7]([CH2:19][OH:20])=[N:6][CH:5]=1.[F:22][C:23]1[CH:30]=[CH:29][C:26]([CH2:27][NH2:28])=[CH:25][CH:24]=1>CN(C)C=O>[CH2:12]([O:11][C:8]1[C:7]([CH2:19][OH:20])=[N:6][CH:5]=[C:4]([C:9]=1[OH:10])[C:3]([NH:28][CH2:27][C:26]1[CH:29]=[CH:30][C:23]([F:22])=[CH:24][CH:25]=1)=[O:21])[C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=1
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참가 물질

4

반응물 2

HCID 673264-FluorobenzylamineHCID 178498811HCID 178498811, 화합물

생성물 1

HCID 178522995HCID 178522995, 화합물수율 72.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
120 °C

실험 절차

The compound 18 (3.76 g, 13.0 mmol) was dissolved in dimethylformamide (38 ml), and 4-fluorobenzylamine (2.44 ml, 21.3 mmol) was added, followed by stirring at 120° C. for 2 hours. The reaction solution was cooled to room temperature, and the solvent was distilled off under reduced pressure, followed by dilution with ethyl acetate. Thereafter, this was washed with 2N hydrochloric acid and water, and dried with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the residue was washed with diethyl ether to obtain 5-benzyloxy-N-(4-fluoro-benzyl)-4-hydroxy-6-hydroxymethyl-nicotinic acid amide 10 (3.59 g, 72%) as a beige crystal.

후처리

  1. temperatureThe reaction solution was cooled to room temperature
  2. distillationthe solvent was distilled off under reduced pressure
  3. washThereafter, this was washed with 2N hydrochloric acid and water
  4. dry with materialdried with anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. washthe residue was washed with diethyl ether

출처 및 근거

ORD 기록
ord-95a7cf67cbe94d8b89567f3b5d403bc3
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07858788B2

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