Photobase generator and photoresist composition containing same
A technology of photoresist and photobase generator, which is applied in photosensitive materials for photomechanical equipment, original parts for photomechanical processing, optics, etc., and can solve problems such as loss of contact holes and pattern collapse
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example 1
[0119] Example 1: Synthesis of NB-DiOC (C)
[0120]
[0121]
[0122] 1,1'-Carbonyldiimidazole (5.3 g; 1.0 eq.) was suspended in anhydrous DMF (60 mL) under nitrogen atmosphere generally as described in Scheme 1 above. The solution was cooled to 0°C and (2-nitrophenyl)methanol (5.0 g; 1.0 eq.) in anhydrous DMF (40 mL) was added slowly. After stirring at RT for 3 hours, dioctylamine (7.88 g; 1.0 eq.) was added. The mixture was stirred at 70°C for 20 hours. The reaction mixture was diluted with EA, washed with water. The organic phase was dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude compound of the title compound was purified by flash chromatography (EtOAc / heptane).
example 2
[0123] Example 2: Synthesis of NB-DEHC (E)
[0124]
[0125] Triphosgene (1.16 g; 0.3 eq.) was suspended in anhydrous DCM (30 mL) under a nitrogen atmosphere generally as described above in Scheme 2. The solution was cooled to 0 °C. Then, (2-nitrophenyl)methanol (2.0 g; 1.0 eq.) and N,N-diisopropylethylamine (3.38 g; 2.0 eq.) in dry DCM (30 mL) were added. After stirring at RT for 3 hours, bis(2-ethylhexyl)amine (3.15 g; 1.0 eq.) was added slowly and it was stirred for 4 hours. The reaction mixture was washed with water and the organic phase was dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude title compound was purified by flash chromatography (EtOAc / heptane).
example 3
[0126] Example 3: Synthesis of ANT-DEHC
[0127]
[0128] Triphosgene (2.137 g; 0.5 eq.) was suspended in anhydrous DCM (30 mL) under a nitrogen atmosphere generally as described in Scheme 3 above. The solution was cooled to 0 °C. Then, 9-(hydroxymethyl)anthracene (3.0 g; 1.0 eq.) and N,N-diisopropylethylamine (3.723 g; 2.0 eq.) in dry DCM (100 mL) were added. After stirring at RT for 3 hours, bis(2-ethylhexyl)amine (3.478 g; 1.0 eq.) was added slowly and it was stirred for 4 hours. The reaction mixture was washed with water and the organic phase was dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude title compound was purified by flash chromatography (EtOAc / heptane).
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