4,4'-二羟基联苯 → Xanthene biphenylene

HRID 2109350

反应方程式

HRID 2109350 反应方程式
C(O[C:6]1[C:19](C)=[C:18](C)[C:17]2[O:16][C:15]3[C:10](=[C:11](C)[C:12](OCC4OC4)=[C:13](C)[C:14]=3C)[CH:9](C3C=CC=CC=3)[C:8]=2[C:7]=1C)C1OC1.C(O[C:42]1[CH:47]=[CH:46][C:45]([C:48]2[CH:53]=[CH:52][C:51](OCC3OC3)=[CH:50][CH:49]=2)=[CH:44][CH:43]=1)C1OC1.OC1C=CC(C2C=CC(O)=CC=2)=CC=1.C([O-])(=O)C.C([P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)C>CN(C)C(=O)C.CO>[CH:11]1[C:10]2[CH2:9][C:8]3[C:17](=[CH:18][CH:19]=[CH:6][CH:7]=3)[O:16][C:15]=2[CH:14]=[CH:13][CH:12]=1.[CH:50]1[C:49]2[C:44]3[C:45](=[CH:46][CH:47]=[CH:42][CH:43]=3)[C:48]=2[CH:53]=[CH:52][CH:51]=1

参与物

7

反应物 4

HCID 71124,4'-二羟基联苯HCID 94470乙基三苯基醋酸膦HCID 1028244,4'-Bis(2,3-epoxypropoxy)biphenylHCID 587469822,7-Diglycidyloxy-1,3,4,5,6,8-hexamethyl-9-phenylxanthene

产物 1

HCID 69049558Xanthene biphenylene收率 95%

试剂、催化剂与溶剂 2

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂HCID 31374N,N-二甲基乙酰胺溶剂2 次

实验过程

1.555 g (manufactured by DAINIPPON INK & CHEMICALS Co., Ltd., “EXA7335”, 3.2 mmol) of 2,7-diglycidyloxy-1,3,4,5,6,8-hexamethyl-9-phenylxanthene, 0.238 g (0.8 mmol) of 4,4′-diglycidyloxybiphenyl, 0.67 g (3.6 mmol) of 4,4′-dihydroxybiphenyl and 0.0106 g (0.02 mmol) of ethyltriphenylphosphonium acetate in a 70% methanol solution were reacted for 4 hours by stirring while heating to 160° C. in 2.463 g of N,N-dimethylacetamide under a nitrogen atmosphere. After cooling, a pale yellow transparent semi-solid reaction solution was diluted with 11.495 g of N,N-dimethylacetamide and then added dropwise in ice. The resulting white massive precipitate was suction-filtered, washed with ice water and then boiled in 200 ml of water for 30 minutes while vigorously stirring. After cooling, the precipitate obtained by decantation was ground and the powered precipitate was washed with water and methanol, and then vacuum dried at 60° C. to obtain a xanthene-biphenylene copolymer type linear epoxy resin. The amount of the resulting xanthene-biphenylene copolymer type linear epoxy resin was 2.33 g and the yield was 95%.

后处理

  1. temperatureAfter cooling
  2. customa pale yellow transparent semi-solid reaction solution
  3. additionadded dropwise in ice
  4. filtrationThe resulting white massive precipitate was suction-filtered
  5. washwashed with ice water
  6. stirringwhile vigorously stirring
  7. temperatureAfter cooling
  8. customthe precipitate obtained by decantation
  9. washthe powered precipitate was washed with water and methanol
  10. customvacuum dried at 60° C.

来源与证据

ORD记录
ord-d968195c09f1446da5e931a071bdfc9f
来源数据集
uspto-grants-2009_04
专利号
US07514507B2

关联笔记

加载中…