2-(2-羟基苯基)苯并恶唑,请磨灭 → HCID 67072674，化合物

HRID 1506817

反应方程式

HRID 1506817 反应方程式
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

参与物

4

反应物 2

HCID 132692-(2-羟基苯基)苯并恶唑,请磨灭HCID 596810二苯基硼酸酐

产物 1

HCID 67072674HCID 67072674，化合物

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂2 次

实验过程

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:

后处理

  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)

来源与证据

ORD记录
ord-0c15ac0549a74bb9b8ae73caa55a46a3
来源数据集
uspto-grants-2015_12
专利号
US09221770B2

关联笔记

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