Benzyl Bromide → HCID 68431966, 화합물

HRID 2267005노트

반응식

HRID 2267005 반응식
[CH2:1](Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I:9][C:10]1[C:15]([OH:16])=[CH:14][CH:13]=[CH:12][C:11]=1O.[C:18](=[O:21])([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[CH2:1]([O:16][C:15]1[CH:14]=[CH:13][CH:12]=[C:11]([O:21][CH2:18][C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:10]=1[I:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 10796Cesium carbonateHCID 6168332-iodobenzene-1,3-diol

생성물 1

HCID 68431966HCID 68431966, 화합물수율 71.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Add benzyl bromide (7.97 g, 46.6 mmol) to a solution of 2-iodo-benzene-1,3-diol (5.00 g, 21.2 mmol) and cesium carbonate (15.2 g, 46.6 mmol) in dimethylformamide (200 mL) and stir. After 18 hours, concentrate under reduced pressure. Add water (500 mL) and stir. After 1 hour, filter the resulting precipitate washing with water and hexanes to yield the title compound as an off-white solid (6.30 g, 71%): 1H NMR (CDCl3) δ 5.18 (s, 4H), 6.55 (d, 2H), 7.19 (t, 1H), 7.29-7.53 (m, 10H).

후처리

  1. concentrationconcentrate under reduced pressure
  2. stirringAdd water (500 mL) and stir
  3. waitAfter 1 hour
  4. filtrationfilter the resulting precipitate
  5. washwashing with water and hexanes

출처 및 근거

ORD 기록
ord-0b9c62b785374723a61f3d84a3e797b8
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07858646B2

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