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 temperature and 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
- 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-9e6cc456a1594546baa447331160c922
- 出典データセット
- uspto-grants-1991_11
- 特許番号
- US05064819
反応ノート
読み込み中…