4,4'-Dihydroxybiphenyl → Xanthene biphenylene

HRID 2109350

反応式

HRID 2109350 の反応式
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

参加物

7

反応物 4

HCID 71124,4'-DihydroxybiphenylHCID 94470Ethyltriphenylphosphonium acetateHCID 1028244,4'-Bis(2,3-epoxypropoxy)biphenylHCID 587469822,7-Diglycidyloxy-1,3,4,5,6,8-hexamethyl-9-phenylxanthene

生成物 1

HCID 69049558Xanthene biphenylene収率 95%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 31374Dimethylacetamide溶媒2 回

実験手順

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%.

後処理

  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.

出典と根拠

ORDレコード
ord-d968195c09f1446da5e931a071bdfc9f
出典データセット
uspto-grants-2009_04
特許番号
US07514507B2

関連ノート

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