Hydrochloric Acid → HCID 9942683、化合物
反応式
[NH2:1][CH2:2][CH2:3][CH2:4][P:5]([CH:8](OCC)OCC)(=[O:7])[OH:6].[CH2:15]([SH:18])[CH2:16][SH:17].Cl>C(O)(=O)C>[NH2:1][CH2:2][CH2:3][CH2:4][P:5]([CH:8]1[S:18][CH2:15][CH2:16][S:17]1)(=[O:7])[OH:6]参加物
5
実験手順
To a solution of 0.90 g (4.0 mmol) of 3-aminopropyl(diethoxymethyl)phosphinic acid in 10 ml of glacial acetic acid at 0° there are added 0.38 ml (4,4 mmol) of ethane-1 2-dithiol, followed by addition of 2 ml of concentrated hydrochloric acid over a period of 5 min. The mixture is allowed to warm to room temperatureand is then stirred for 18 hours. After removal of acetic and hydrochloric acids under high vacuum, the residue is chromatographed (Opti-Up® C12 50%, water) and recrystallized from methanol to yield 3-aminopropyl(1,3-dithiolan-2-yl)phosphinic acid, m.p. 272°-274°.
後処理
- temperatureto warm to room temperatureand
- customAfter removal of acetic and hydrochloric acids under high vacuum
- customthe residue is chromatographed (Opti-Up® C12 50%, water)
- customrecrystallized from methanol
出典と根拠
- ORDレコード
- ord-034d2520cb4345009bcfc20c35b7543a
- 出典データセット
- uspto-grants-1991_09
- 特許番号
- US05051524
反応ノート
読み込み中…