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Bromine → HCID 10192904, 화합물

HRID 1836795
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HRID 1836795 반응식
[Br-:1].[K+].BrBr.[C:5]([O:8][C:9]1[C:16]([O:17][CH3:18])=[CH:15][CH:14]=[CH:13][C:10]=1[CH:11]=[O:12])(=[O:7])[CH3:6]>O>[C:5]([O:8][C:9]1[C:16]([O:17][CH3:18])=[CH:15][CH:14]=[C:13]([Br:1])[C:10]=1[CH:11]=[O:12])(=[O:7])[CH3:6]
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참가 물질

5

반응물 3

HCID 24408BromineHCID 2517032-Acetoxy-3-methoxybenzaldehydeHCID 253877Potassium Bromide

생성물 1

HCID 10192904HCID 10192904, 화합물수율 79%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of potassium bromide (40 g) in H2O (250 mL) was added bromine (6.8 mL). To the dark red solution was added aldehyde 10 (20.2 g). The turbid orange solution was stirred overnight, filtered, rinsed with ethyl acetate, recrystallized from ethyl acetate/hexane to afford yellow crystals (22.4 g, 79%): m.p. 121.6-123.4° C., lit18 m.p. 119-120° C.; EIMS m/z 274 (M+, 81Br), 272 (M+, 79Br), 232, 230, 186, 184, 43; 1H NMR δ 10.26 (1H, s, CHO), 7.51 (1H, d, J=9.0 Hz, H4), 7.05 (1H, d, J=9.0 Hz H2, H4), 3.85 (3H, s, OCH3), 2.38 (3H, s, COCH3); 13C—NMR (75.5 MHZ) δ 190.38, 168.71, 151.78, 140.37, 131.41, 126.49, 117.69, 116.35, 56.40, 20.44. Anal. Calcd. For C10H9O4Br: C, 43.98; H, 3.32. Found: C, 44.46; H, 3.55.

후처리

  1. filtrationfiltered
  2. washrinsed with ethyl acetate
  3. customrecrystallized from ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-432065092de1456f9baeace584818f96
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06777578B2

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