Sodium sulfate decahydrate → 3-(5-Methyl-2-phenyl-4-thiazolylmethoxy)-5-isoxazolylmethanol

HRID 1294187노트

반응식

HRID 1294187 반응식
[CH3:1][C:2]1[S:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:19]=[C:18]([C:20](OC)=[O:21])[O:17][N:16]=1.[H-].C([Al+]CC(C)C)C(C)C.O.O.O.O.O.O.O.O.O.O.[O-]S([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:1][C:2]1[S:6][C:5]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:19]=[C:18]([CH2:20][OH:21])[O:17][N:16]=1

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 17861290Methyl 3-(5-methyl-2-phenyl-4-thiazolylmethoxy)-5-isoxazolecarboxylateHCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 178613523-(5-Methyl-2-phenyl-4-thiazolylmethoxy)-5-isoxazolylmethanol수율 80.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

To a solution of methyl 3-(5-methyl-2-phenyl-4-thiazolylmethoxy)-5-isoxazolecarboxylate (5.27 g) in tetrahydrofuran (100 ml) was slowly added diisobutylaluminum hydride (0.95 M hexane solution, 60 ml) at 0° C. and the mixture was stirred at 0° C. for 1 hr. Sodium sulfate 10 hydrate (17.01 g) was added to the reaction mixture and the mixture was further stirred at room temperature for 30 min. The insoluble materials were removed by filtration, and the filtrate was concentrated to give [3-(5-methyl-2-phenyl-4-thiazolylmethoxy)-5-isoxazolyl]methanol (3.88 g, 80%) as colorless crystals. The crystals were recrystallized from ethyl acetate-hexane. melting point: 84-85° C.

후처리

  1. customat 0° C.
  2. stirringthe mixture was further stirred at room temperature for 30 min
  3. customThe insoluble materials were removed by filtration
  4. concentrationthe filtrate was concentrated

출처 및 근거

ORD 기록
ord-34e5e3aea3614ad1a576d81527a06ca3
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07238716B2

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