Hydrochloric Acid → HCID 10279881, 화합물

HRID 1247625노트

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HRID 1247625 반응식
[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+].Cl>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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 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

생성물 1

HCID 10279881HCID 10279881, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
-5 °C

실험 절차

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 hydrochloric 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°.

후처리

  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

출처 및 근거

ORD 기록
ord-68db64d4da9b4f248a4e67a63a4e0f5a
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129352B2

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