関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Squaric acid | HCID 17913 | — |
| 反応物 | Distearylperimidine | HCID 131734169 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | Squaric Acid Distearylperimidine | HCID 131734168 | 78% |
反応手順
To a 100 ml round bottom flask equipped with Teflon coated stir magnetic and a condenser was charged 2.0 g squaric acid (MW=114), 50 g toluene and 50 g butanol. The round bottom flask was placed in an 80° C. to 90° C. oil bath. After the squaric acid dissolved, 22.3 g distearylperimidine (MW=635) was added. The reaction progress was monitored by uv-vis spectrum, the results of which are illustrated in FIG. 1. The peak at about 811 nm grew and the peak at 355 decreased. After 3.5 hours the absorbance ratio at 811 nm to 355 nm reached the max 11.62. The reaction mixture was quenched in about 400 ml methanol after 5 hrs of reaction. Sticky solids came out and were filtered and rinsed with more methanol three times. The very sticky solids were dissolved in THF and subsequently dried. The yield was about 78%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09193869B2 |
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| 出典データセット | uspto-grants-2015_11 |
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| ORD ID | ord-3570a66d524e4e678224a4bac3413148 |
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| 出典メモ | uspto-grants-2015_11 |
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