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Sodium Sulfate → (S)-1-(2-hydroxypropyl)-5-methyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid

HRID 2356360
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HRID 2356360 반응식
[CH3:1][C:2]1[NH:6][N:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[C:4](=[O:13])[C:3]=1[C:14]([O:16]CC1C=CC=CC=1)=[O:15].C[Al](C)C.[CH3:28][C@H:29]1[CH2:31][O:30]1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+].S([O-])([O-])(=O)=O.[Na+].[Na+]>C1COCC1.ClC1C=CC=CC=1>[OH:30][C@@H:29]([CH3:31])[CH2:28][N:6]1[C:2]([CH3:1])=[C:3]([C:14]([OH:16])=[O:15])[C:4](=[O:13])[N:5]1[C:7]1[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1
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참가 물질

8

반응물 5

HCID 24436Sodium SulfateHCID 62649Sodium sulfate decahydrateHCID 146262(2S)-2-MethyloxiraneHCID 16682925TrimethylaluminumHCID 24886175Benzyl 5-methyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylate

생성물 1

HCID 59383933
(S)-1-(2-hydroxypropyl)-5-methyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylic acid
수율 54.3%

시약·촉매·용매 2

HCID 7964Chlorobenzene용매HCID 8028Tetrahydrofuran용매

실험 절차

To a 500 mL round-bottomed flask was added benzyl 5-methyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxylate (3.1 g, 10 mmol), chlorobenzene (30 mL) and the mixture cooled in an ice bath. The trimethylaluminum (25 ml, 50 mmol) was added and the ice bath removed followed by the addition of (S)-2-methyloxirane (0.87 g, 15 mmol). The mixture stirred 1 h and cooled in an ice bath with the addition of THF (60 mL). Sodium sulfate decahydrate (3g) was added to the mixture cautiously (foaming) and the mixture stirred 1 h. Sodium sulfate (10 g) was added and stirred 1 h. The mixture was filtered through celite, washed with 4:1 chloroform/isopropanol and the filtrate concentrated, diluted with chloroform, washed with 1 N HCl and sat. sodium bicarbonate. The organic layer was dried over sodium sulfate and concentrated. The crude product was purified by silica gel chromatography eluting with methanol/chloroform to afford the title compound as a foam (1.5 g). MS (ESI pos. ion) m/z: 367 (MH+). Calc'd exact mass for C21H22N2O4: 366.

후처리

  1. temperaturethe mixture cooled in an ice bath
  2. customthe ice bath removed
  3. stirringthe mixture stirred 1 h
  4. stirringstirred 1 h
  5. filtrationThe mixture was filtered through celite
  6. washwashed with 4:1 chloroform/isopropanol
  7. concentrationthe filtrate concentrated
  8. additiondiluted with chloroform
  9. washwashed with 1 N HCl and sat. sodium bicarbonate
  10. dry with materialThe organic layer was dried over sodium sulfate
  11. concentrationconcentrated
  12. customThe crude product was purified by silica gel chromatography
  13. washeluting with methanol/chloroform

출처 및 근거

ORD 기록
ord-160a8be336344c218c357b80122f5722
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07759344B2

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