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1,2-Benzenedimethanol → N,N-Diisopropyl-1,5-dihydrobenzo[e][1,3,2]dioxaphosphepin-3-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Benzenedimethanol | HCID 69153 | — |
| 反応物 | Bis(diisopropylamino)chlorophosphine | HCID 2733425 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N,N-Diisopropyl-1,5-dihydrobenzo[e][1,3,2]dioxaphosphepin-3-amine | HCID 19782585 | — |
反応手順
Phthalyl alcohol (1.15 g, 8.31 mmol) was dissolved in 5 ml of THF, and bisdiisopropylaminochlorophosphine (2.21 g, 8.31 mmol) which was dissolved in 5 ml of THF was added dropwise to the solution at -15° C. under a nitrogen atmosphere. Afterward, the temperature of the solution was adjusted to room temperature, and after the disappearance of phthalyl alcohol had been confirmed, hydrochloride of diisopropylamine was washed with ether. The wash liquor was concentrated and then distilled in order to obtain the desired product having a melting point of from 150° to 155° C. (0.7 mmHg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05264605 |
| 出典データセット | uspto-grants-1993_11 |
| ORD ID | ord-9d568a1daaed4c6d917cab90fc95f644 |
| 出典メモ | uspto-grants-1993_11 |