Sodium Carbonate → HCID 19077476、化合物

HRID 964566

反応式

HRID 964566 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 19077476HCID 19077476、化合物

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

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+).

後処理

  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%)

出典と根拠

ORDレコード
ord-371d0e347a4640b38d6a9dc5fcac741b
出典データセット
uspto-grants-1998_06
特許番号
US05770598

関連ノート

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