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Phenethylamine → 4-chloro-N-(2-phenylethyl)butanamide

HRID 521741
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HRID 521741 반응식
[CH2:1]([NH2:9])[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[OH-].[Na+].[Cl:12][CH2:13][CH2:14][CH2:15][C:16](Cl)=[O:17]>C(Cl)Cl.O>[Cl:12][CH2:13][CH2:14][CH2:15][C:16]([NH:9][CH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1)=[O:17]
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참가 물질

5

반응물 3

HCID 1001PhenethylamineHCID 14798Sodium HydroxideHCID 783704-Chlorobutyryl chloride

생성물 1

HCID 51423824-chloro-N-(2-phenylethyl)butanamide수율 93%

시약·촉매·용매 1

HCID 21908982Water methylene chloride용매

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온도
0 °C

실험 절차

To a solution of phenethylamine (2.42 g, 20 mmol) and NaOH (0.88 g, 22 mmol) in DCM/H2O (20 mL/20 mL) was added 4-chloro-butyryl chloride (2.82 g, 20 mmol) at 0° C. The resulting mixture was stirred at 0° C. for 20 min. The mixture was partitioned between DCM (20 mL) and H2O (10 mL). The organic layer was separated and washed with brine (10 mL), dried over anhydrous Na2SO4, filtered and concentrated to give a white solid. This residue was purified with silica gel column (Hexane/EtOAc=3/1 to 1/1) to obtain HJC-1-48 (4.2 g, 93%) as a white solid. 1H NMR (600 MHz, CDCl3) δ 7.32 (t, 2H, J=7.8 Hz), 7.23-7.26 (m, 1H), 7.20 (d, 2H, J=7.8 Hz), 5.46-5.47 (m, 1H), 3.52-3.58 (m, 4H), 2.82 (t, 2H, J=7.2 Hz), 2.31 (t, 2H, J=7.2 Hz), 2.07-2.11 (m, 2H).

후처리

  1. customThe mixture was partitioned between DCM (20 mL) and H2O (10 mL)
  2. customThe organic layer was separated
  3. washwashed with brine (10 mL)
  4. dry with materialdried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give a white solid
  8. customThis residue was purified with silica gel column (Hexane/EtOAc=3/1 to 1/1)

출처 및 근거

ORD 기록
ord-a32028168ab8480fb934388a994bb12b
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09328125B2

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