Hydrochloric Acid → HCID 9942683, 화합물
반응식
[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]참가 물질
5
실험 절차
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°.
후처리
- customAfter removal of acetic and hydrochloric acids under high vacuum
- customthe residue is chromatographed (Opti-Up® C12 50%, water)
- customrecrystallized from methanol
출처 및 근거
- ORD 기록
- ord-9e6cc456a1594546baa447331160c922
- 출처 데이터셋
- uspto-grants-1991_11
- 특허 번호
- US05064819
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