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Diisopropylethylamine → HCID 178485964、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-Chlorophenyl chloroformate | HCID 139059 | — |
| 反応物 | HCID 178484804 | HCID 178484804 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | KHSO4 ether | HCID 86584777 | — |
| 生成物 | HCID 178485964 | HCID 178485964 | 117.5% |
反応手順
A solution of 1.41 g (corresponds to 3.0 mmol) of trans-Methanesulfonic acid 3-(4-methylamino-cyclohexyl)-prop-2-ynyl ester trifluoroacetate in 20 ml CH2Cl2 was first cooled at 0° C., treated with 0.5 ml (3.6 mmol) 4-chlorophenylchloroformate and then with 2.57 ml (15 mmol; 5 equivalents) of Huenigs base (during 3 min). After 45 min at RT, the mixture was dissolved in aqueous 10% KHSO4/Et2O (3×). The organic phases were washed with aqueous 10% NaCl, dried over Na2SO4 and evaporated to give 1.41 g (quantitative) of crude trans-Methanesulfonic acid 3-{4-[(4-chloro-phenoxycarbonyl)-methyl-amino]-cyclohexyl}-prop-2-ynyl ester, MS: 400 (MH+, 1Cl). The crude product was directly used in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07335687B2 |
| 出典データセット | uspto-grants-2008_02 |
| ORD ID | ord-961ae6a25a3c480a9cb7188510020e34 |
| 出典メモ | uspto-grants-2008_02 |