Sodium Carbonate → HCID 19077476, 화합물

HRID 964566

반응식

HRID 964566 반응식
[CH3:1][C:2]1[C:7]2[O:8][C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=3[C:6]=2[CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[Na+].[Na+].[Br:21]Br>CCCCCC>[Br:21][C:3]1[CH:4]=[CH:5][C:6]2[C:10]3[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=3[O:8][C:7]=2[C:2]=1[CH3:1]

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 24408BromineHCID 43489Dibenzofuran, 4-methyl-

생성물 1

HCID 19077476HCID 19077476, 화합물

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

4-Methyldibenzofuran (30 g, 165 mmol) and sodium carbonate (17.5 g, 165 mmol) were mixed in hexane (300 ml) and bromine (26.4 g, 165 mmol) was added. The reaction was stirred at room temperature for 72 hours, then the solvent was removed in vacuo to give an oil which crystallised. Recrystallisation from IMS yielded several batches of off-white crystals (31.22 g, 72%) with m.p. 124°-125° C. (Found: C, 58.59; H, 3,28. C13H9BrO 0.31H2O requires: C, 58.58; H, 3.63%); δH [2H6 ]-DMSO 8.15 (1H, d), 7.9 (1H, d), 7.7 (1H, d), 7.4 (1H, t), 7.05 (2H, m), 2.6 (3H, s); m/z 260/262 (M+).

후처리

  1. customthe solvent was removed in vacuo
  2. customto give an oil which
  3. customcrystallised
  4. customRecrystallisation from IMS yielded several batches of off-white crystals (31.22 g, 72%) with m.p. 124°-125° C. (Found: C, 58.59; H, 3,28. C13H9BrO 0.31H2O requires: C, 58.58; H, 3.63%)

출처 및 근거

ORD 기록
ord-371d0e347a4640b38d6a9dc5fcac741b
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05770598

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