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Magnesium Hydroxide → HCID 24821555、化合物

HRID 2064101
ノート
印刷プレビュー

反応式

HRID 2064101 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 73981Magnesium HydroxideHCID 24763648HCID 24763648、化合物

生成物 1

HCID 24821555HCID 24821555、化合物収率 92%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
7.5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-06043520684f4df5aafbf3a4e7787ad5
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08288416B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート