化工社化工社 化学情報印刷レポート · 研究参考用
Acetonitrile → Carbonic acid 2,5-dioxo-pyrrolidin-1-yl ester 2-(2-hexadecyl-2,5,7,8-tetramethyl-chroman-6-yloxy)-ethyl Ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Di(succinimido) carbonate | HCID 676246 | — |
| 反応物 | 2-(2-Hexadecyl-2,5,7,8-tetramethyl-chroman-6-yloxy)-ethanol | HCID 59347262 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Carbonic acid 2,5-dioxo-pyrrolidin-1-yl ester 2-(2-hexadecyl-2,5,7,8-tetramethyl-chroman-6-yloxy)-ethyl Ester | HCID 59347260 | 77% |
反応手順
Compound 17 (10.5 g, 22 mmol) was dissolved in anhydrous dichloromethane (150 mL). To the solution were added disuccinimidyl carbonate (8.45 g, 33 mmol), triethylamine (20 mL) and acetonitrile (50 mL). The reaction mixture was stirred at room temperature under argon for over night and then evaporated dryness. The residue was dissolved in dichloromethane (300 mL). It was washed with saturated NaHCO3 aqueous solution (3×100 mL). The organic layer was dried over Na2SO4, filtered and evaporated to dryness. Compound 18 (10.4 g, 77%) was obtained as colorless powder after drying in high vacuum, which was directly used for the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09394540B2 |
| 出典データセット | uspto-grants-2016_07 |
| ORD ID | ord-b646edae397e4e37919abe750a39deba |
| 出典メモ | uspto-grants-2016_07 |