Dimethyl Sulfate → HCID 70004538, 화합물

HRID 580899노트

반응식

HRID 580899 반응식
S([O:6][CH3:7])(OC)(=O)=O.Cl.O[C:10]1[C:15]2=[N:16][C:17]([CH3:24])=[C:18]([CH2:21][CH2:22][OH:23])[C:19](=[O:20])[N:14]2[CH:13]=[CH:12][CH:11]=1.[OH-].[Na+]>O>[OH:23][CH2:22][CH2:21][C:18]1[C:19](=[O:20])[N:14]2[CH:13]=[CH:12][CH:11]=[C:10]([O:6][CH3:7])[C:15]2=[N:16][C:17]=1[CH3:24]

참가 물질

5

반응물 3

HCID 6497Dimethyl SulfateHCID 14798Sodium HydroxideHCID 468523699-Hydroxy-3-(2-hydroxyethyl)-2-methyl-4h-pyrido[1,2-a]pyrimidin-4-onehydrochloride

생성물 1

HCID 70004538HCID 70004538, 화합물수율 49.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Dimethyl sulfate (2.52 g) was added dropwise to a mixture of intermediate 9 (4.4 g) and sodium hydroxide (0.8 g) in water (10 ml), while cooling in ice water. The reaction mixture was stirred for 15 minutes at RT, then it was heated for 1 hour using a warm water bath. The reaction mixture was cooled and extracted with CH2Cl2. The precipitate in the separated aqueous layer was filtered off and purified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH 97/3). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from CH3CN. The crystals were filtered off and dried, yielding 2 g (42%) of 3-(2-hydroxyethyl)-9-methoxy-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (intermediate 10).

후처리

  1. temperatureit was heated for 1 hour
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with CH2Cl2
  4. filtrationThe precipitate in the separated aqueous layer was filtered off
  5. custompurified by column chromatography over silica gel (eluent: CH2Cl2 /CH3OH 97/3)
  6. customThe pure fractions were collected
  7. customthe solvent was evaporated
  8. customThe residue was crystallized from CH3CN
  9. filtrationThe crystals were filtered off
  10. customdried

출처 및 근거

ORD 기록
ord-4310c12bec8d4cfca5164fd6c581ebd4
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05919788

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