Compound, resin, material for forming underlayer film for lithography, underlayer film for lithography, pattern forming method, and method for purifying compound or resin
A compound and lower-layer technology, applied in the preparation of organic compounds, chemical instruments and methods, and photosensitive materials for optomechanical equipment, etc., can solve the problems of difficult to obtain resist pattern film thickness, resist pattern collapse, resolution, etc. question
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Embodiment 1
[0310] (Example 1) Synthesis of TriF-3
[0311] Prepare a container with an internal volume of 1000 mL including a stirrer, condenser, and burette. In this container, 100 g (537 mmol) of 4,4-biphenol (reagent manufactured by Tokyo Chemical Industry Co., Ltd.), 49 g (269 mmol) of 4-biphenylaldehyde (manufactured by Mitsubishi Gas Chemical Co., Ltd.) and 400 mL of butyl acetate were added, and concentrated sulfuric acid (96 Mass %, 27 g (269 mmol) of reagent manufactured by Kanto Chemical Co., Ltd., to prepare a reaction liquid. This reaction liquid was stirred at 130°C for 5 hours to perform the reaction. Then, 2 L of ion-exchange water was added to the reaction liquid to precipitate the reaction product, and it was cooled to room temperature. Then, 89 g (534 mmol) of sodium hydroxide aqueous solution (24% by mass) was added, neutralized, and separated by filtration. After drying the solid obtained by filtration, it was dissolved in 400 mL of ethyl acetate, and 400 mL of heptan...
Embodiment 2
[0322] (Example 2) Synthesis of TriF-2
[0323] 100 g of (TriF-3) synthesized in Example 1 was separated by column chromatography to obtain 11.3 g of the target compound group (TriF-2) represented by the following formula.
[0324] It should be noted that through 400MHz- 1 H-NMR found the following peaks.
[0325] 1 H-NMR: (d-DMSO, internal standard TMS)
[0326] δ(ppm) 9.3~9.4(6.1H, O-H), 6.7~7.7(38.8H, Ph-H), 6.0~6.2(2.1H, C-H)
[0327] In addition, the peaks shown in Table 2 and the corresponding molecular weights were observed in LC-MS.
[0328] [Table 2]
[0329] Hold time (minutes)
Molecular weight (m / z)
area(%)
4.79
886.3
94.5
6.36
1236.5
5.5
[0330] From the above 1 The results of H-NMR and LC-MS confirmed that the target compound group obtained in Example 2 is a mixture having a chemical structure of the following formula.
[0331]
[0332] n=1 (94.5%), n=2 (5.5%)
[0333] (TriF-2)
Embodiment 3
[0334] (Example 3) Synthesis of TriF-1
[0335] 10 g of (TriF-2) synthesized in Example 2 was separated by column chromatography to obtain 8.4 g of the target compound (TriF-1) represented by the following formula.
[0336] It should be noted that through 400MHz- 1 H-NMR found the following peaks.
[0337] 1 H-NMR: (d-DMSO, internal standard TMS)
[0338] δ(ppm) 9.3(6H, O-H), 6.7~7.7(38H, Ph-H), 6.0~6.1(2H, C-H)
[0339] In addition, the peaks shown in Table 3 and the corresponding molecular weights were observed in LC-MS.
[0340] [table 3]
[0341] Hold time (minutes)
Molecular weight (m / z)
area(%)
4.79
886.3
>99.8
[0342] From the above 1 The results of H-NMR and LC-MS confirmed that the target compound obtained in Example 3 is a compound having a chemical structure of the following formula.
[0343]
PUM
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