Hydrochloric Acid → HCID 10303884, 화합물

HRID 1760158노트

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HRID 1760158 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.[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])[C:5]1[CH:6]=[CH:7][CH:2]=[CH:3][CH:4]=1

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 10303884HCID 10303884, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
30 °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 (40 ml) was cooled to −5° C. and 1M hydrochloric acid (9.5 ml) containing sodium chloride (7.1 g) was added to adjusted the pH to 3.8. The aqueous phase was separated off and acetonitrile (70 ml) was added to the organic phase. Benzylamine (1.4 ml) was added and 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 benzylammonium (E)-7-[4-(4-fluorophenyl)-6-isopropyl-2-[methyl(methylsulfonyl)amino]pyrimidin-5-yl]-(3R,5S)-3,5-dihydroxyhept-6-enoate (4.4 g) as white crystals. The X-ray powder diffraction spectra for a typical sample of the crystalline benzylammonium salt is shown in FIG. 6 hereinafter. The ten most prominent peaks in the XRD occur at about 2-theta=6.1, 6.7, 16.8, 17.6, 18.1, 19.3, 21.1, 21.9, 23.0 and 26.8°.

후처리

  1. additionwas added
  2. customThe aqueous phase was separated off
  3. additionacetonitrile (70 ml) was added to the organic phase
  4. additionBenzylamine (1.4 ml) was added
  5. customThe product was isolated by filtration at 0° C.
  6. customdried at 35° C. under vacuum

출처 및 근거

ORD 기록
ord-e07902b540134f8190921b24f9392cb1
출처 데이터셋
uspto-grants-2005_01
특허 번호
US06841554B2

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