2-(2-Benzoxazolyl)phenol → 2-(2-Diphenylboroxy phenyl)benzoxazole

HRID 1506817

反応式

HRID 1506817 の反応式
C1(B([O:14][B:15]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)C2C=CC=CC=2)C=CC=CC=1.O[C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=1[C:35]1[O:36][C:37]2[CH:43]=[CH:42][CH:41]=[CH:40][C:38]=2[N:39]=1>O1CCCC1>[C:22]1([B:15]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[O:14][C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=2[C:35]2[O:36][C:37]3[CH:43]=[CH:42][CH:41]=[CH:40][C:38]=3[N:39]=2)[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=1

参加物

4

反応物 2

HCID 132692-(2-Benzoxazolyl)phenolHCID 596810Diphenylborinic anhydride

生成物 1

HCID 670726742-(2-Diphenylboroxy phenyl)benzoxazole

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of diphenylborinic anhydride (5.0 g; 0.014 mole) in tetrahydrofuran (20 ml) was added to a solution of 2-(2′-hydroxyphenyl)benzoxazole (3.1 g; 0.014 mole) in tetrahydrofuran (10 ml). The reaction mixture was refluxed under nitrogen for 2 h and allowed to cool to room temperature, then kept in the refrigerator for 18 h. The product was filtered off under suction, washed with methanol and dried under vacuum at 80° C. for 6 h. Yield 4.4 g (84%). The product was further purified by sublimation (85%). M.p 195° C. (DSC, onset); Tg 59° C. Elemental analysis:

後処理

  1. temperatureThe reaction mixture was refluxed under nitrogen for 2 h
  2. filtrationThe product was filtered off under suction
  3. washwashed with methanol
  4. customdried under vacuum at 80° C. for 6 h
  5. customThe product was further purified by sublimation (85%)
  6. customM.p 195° C. (DSC, onset)

出典と根拠

ORDレコード
ord-0c15ac0549a74bb9b8ae73caa55a46a3
出典データセット
uspto-grants-2015_12
特許番号
US09221770B2

関連ノート

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