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Magnesium Hydroxide → HCID 24821555, 화합물

HRID 2064101
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HRID 2064101 반응식
[C:1]([NH:4][CH2:5][C@@H:6]1[O:10][C:9](=[O:11])[N:8]([C:12]2[CH:17]=[C:16]([F:18])[C:15]([N:19]3[CH2:24][CH2:23][C:22]([O:28][P:29](=[O:32])([OH:31])[OH:30])([CH2:25][O:26][CH3:27])[CH2:21][CH2:20]3)=[C:14]([F:33])[CH:13]=2)[CH2:7]1)(=[O:3])[CH3:2].[OH-].[Mg+2:35].[OH-]>O>[Mg+2:35].[C:1]([NH:4][CH2:5][C@@H:6]1[O:10][C:9](=[O:11])[N:8]([C:12]2[CH:17]=[C:16]([F:18])[C:15]([N:19]3[CH2:24][CH2:23][C:22]([O:28][P:29](=[O:30])([O-:31])[O-:32])([CH2:25][O:26][CH3:27])[CH2:21][CH2:20]3)=[C:14]([F:33])[CH:13]=2)[CH2:7]1)(=[O:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 73981Magnesium HydroxideHCID 24763648HCID 24763648, 화합물

생성물 1

HCID 24821555HCID 24821555, 화합물수율 92%

시약·촉매·용매 1

HCID 962Water용매

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온도
7.5 °C

실험 절차

To a solution of phosphoric acid mono-(1-{4-[(S)-5-(acetylamino-methyl)-2-oxo-oxazolidin-3-yl]-2,6-difluorophenyl}-4-methoxymethyl-piperidin-4-yl)ester (5.0 g, 0.010mol) anhydrous methanol (50 ml) at 0-5° C., under argon, was added powdered anhydrous magnesium hydroxide (0.585 g, 0.010 mol) and water (5 ml) simultanously. The reaction mixture was stirred at 5-10° C. for 2 hours. The ice-bath was removed and the stirring continued further at 30-35° C. for 1 hour. The reaction mixture was filtered and the filtrate evaporated under reduced pressure. Acetone (25 ml) was added to the residue and triturated. The solvent was decanted. This procedure was repeated twice with acetone (50 ml). Acetone after the third trituration was decanted and the residue dried under reduced pressure to obtain the product as white solid, 4.9 g, in 92% yield, Mp>200° C. (dec); MF: C19H24F2MgN3O8P. Aqueous solubility at pH 7 was ˜2 mg/ml.

후처리

  1. customThe ice-bath was removed
  2. waitthe stirring continued further at 30-35° C. for 1 hour
  3. filtrationThe reaction mixture was filtered
  4. customthe filtrate evaporated under reduced pressure
  5. additionAcetone (25 ml) was added to the residue
  6. customtriturated
  7. customThe solvent was decanted
  8. customAcetone after the third trituration was decanted
  9. customthe residue dried under reduced pressure

출처 및 근거

ORD 기록
ord-06043520684f4df5aafbf3a4e7787ad5
출처 데이터셋
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08288416B2

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