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Benzyl Bromide → Ethyl 2-[4-benzyloxy-2-nitronaphthalen-1-yl]acetate

HRID 431744
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HRID 431744 반응식
C([O-])([O-])=O.[K+].[K+].[OH:7][C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])=[C:10]([N+:24]([O-:26])=[O:25])[CH:9]=1.[CH2:27](Br)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>CC(C)=O>[CH2:27]([O:7][C:8]1[C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[C:11]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])=[C:10]([N+:24]([O-:26])=[O:25])[CH:9]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1
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참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 11403107Ethyl 2-[4-hydroxy-2-nitronaphthalen-1-yl]acetate

생성물 1

HCID 11222306Ethyl 2-[4-benzyloxy-2-nitronaphthalen-1-yl]acetate수율 63%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

Anhydrous K2CO3 (0.50 g, 3.68 mmol) was added to a solution of ethyl 2-[4-hydroxy-2-nitronaphthalen-1-yl]acetate (0.42 g, 1.53 mmol) and benzyl bromide (0.44 mL, 3.68 mmol) in acetone (4 mL) at room temperature, and the mixture was stirred overnight. The reaction mixture was filtered, and the filtrate was concentrated. The residue was diluted with AcOEt (50 mL), and to the mixture was added N-methypiperazine (3 mL) to remove any excess benzyl bromide. The mixture was washed with water (10 mL), 1 M HCl (10 mL), saturated aqueous NaHCO3 (10 mL) and saturated aqueous NaCl (10 mL), and then dried (Na2SO4) and evaporated to yield ethyl 2-[4-benzyloxy-2-nitronaphthalen-1-yl]acetate (0.35 g, 63%) as a yellow solid. Mp 128-130° C.; 1H NMR (CDCl3, 500 MHz) δ 8.44 (dd, 0.5, 8.0, 1H), 8.10 (d, 8.5, 1H), 7.71 (t, 7.0, 1H), 7.66 (t, 7.0, 1H), 7.54 (d, 7.0, 2H), 7.46 (t, 7.5, 2H), 7.43 (s, 1H), 7.40 (t, 7.0, 1H), 5.32 (s, 2H), 4.33 (s, 2H), 4.21 (q, 7.0, 2H), 1.27 (t, 7.0, 3H); EIMS m/z 365 (M+); IR (neat) νmax 2980, 1725, 1592, 1524, 1512, 1469, 1451, 1426, 1371, 1331, 1252, 1202, 1159, 1111, 1022, 842, 770, 756, 724, 690 cm−1.

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. additionThe residue was diluted with AcOEt (50 mL)
  4. additionto the mixture was added N-methypiperazine (3 mL)
  5. customto remove any excess benzyl bromide
  6. washThe mixture was washed with water (10 mL), 1 M HCl (10 mL), saturated aqueous NaHCO3 (10 mL) and saturated aqueous NaCl (10 mL)
  7. dry with materialdried (Na2SO4)
  8. customevaporated

출처 및 근거

ORD 기록
ord-1f38b9929a1c4bbc98e7f590a87fb850
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06660742B2

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