Sodium Chloride → HCID 10279881、化合物

HRID 1760157ノート

反応式

HRID 1760157 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13](/[CH:14]=[CH:15]/[C@@H:16]([OH:24])[CH2:17][C@@H:18]([OH:23])[CH2:19][C:20]([O-:22])=[O:21])=[C:12]([CH:25]([CH3:27])[CH3:26])[N:11]=[C:10]([N:28]([CH3:33])[S:29]([CH3:32])(=[O:31])=[O:30])[N:9]=2)=[CH:4][CH:3]=1.[Na+].[Cl-].[Na+]>C(#N)C>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:13](/[CH:14]=[CH:15]/[C@@H:16]([OH:24])[CH2:17][C@@H:18]([OH:23])[CH2:19][C:20]([O-:22])=[O:21])=[C:12]([CH:25]([CH3:27])[CH3:26])[N:11]=[C:10]([N:28]([CH3:33])[S:29]([CH3:32])(=[O:31])=[O:30])[N:9]=2)=[CH:4][CH:3]=1.[CH2:8]([NH3+:9])[CH3:5]

参加物

4

反応物 2

HCID 5234Sodium ChlorideHCID 23684378sodium (3R,5S,6E)-7-(4-(4-fluorophenyl)-2-(N-methylmethanesulfonamido)-6-(propan-2-yl)pyrimidin-5-yl)-3,5-dihydroxyhept-6-enoate

生成物 1

HCID 10279881HCID 10279881、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
-5 °C

実験手順

A solution of sodium (E)-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl]-(3R,5S)-3,5-dihydroxyhept-6-enoate in aqueous acetonitrile (11 ml) containing sodium chloride (1.4 g) was cooled to −5° C. and the pH adjusted to 3.4 to 4 with 1M hydrchloric acid. The aqueous phase was separated off and the organic phase was filtered through anhydrous magnesium sulphate. Acetonitrile (14 ml) was added to the organic phase and aqueous ethylamine (0.21 ml) was added. The solution was heated to 30° C. and held at this temperature for 90 minutes. The product was isolated by filtration at 0° C. and dried at 35° C. under vacuum to give ethylammonium (E)-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl]-(3R,5S)-3,5-dihydroxyhept-6-enoate (0.7 g) as white crystals. The X-ray powder diffraction spectra for a typical sample of the crystalline ethylammonium salt is shown in FIG. 3 hereinafter. The ten most prominent peaks in the XRD occur at about 2-theta=8.6, 15.9, 16.9, 18.4, 18.7, 19.7, 20.8, 23.3, 23.8 and 25.8°.

後処理

  1. customThe aqueous phase was separated off
  2. filtrationthe organic phase was filtered through anhydrous magnesium sulphate
  3. additionAcetonitrile (14 ml) was added to the organic phase and aqueous ethylamine (0.21 ml)
  4. additionwas added
  5. temperatureThe solution was heated to 30° C.
  6. customThe product was isolated by filtration at 0° C.
  7. customdried at 35° C. under vacuum

出典と根拠

ORDレコード
ord-4f83adf925a044b1bfeb6f30eb362d98
出典データセット
uspto-grants-2005_01
特許番号
US06841554B2

反応ノート

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