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 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°.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-034d2520cb4345009bcfc20c35b7543a
- 출처 데이터셋
- uspto-grants-1991_09
- 특허 번호
- US05051524
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