Sodium sulfate decahydrate → 3-Ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl alcohol

HRID 1295215노트

반응식

HRID 1295215 반응식
C([O:3][C:4](=O)[C:5]1[CH:10]=[C:9]([O:11][CH2:12][C:13]2[N:14]=[C:15]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[O:16][C:17]=2[CH3:18])[CH:8]=[C:7]([O:25][CH2:26][CH3:27])[CH:6]=1)C.[H-].[Li+].[Al+3].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.[O-]S([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH2:26]([O:25][C:7]1[CH:6]=[C:5]([CH:10]=[C:9]([O:11][CH2:12][C:13]2[N:14]=[C:15]([C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=3)[O:16][C:17]=2[CH3:18])[CH:8]=1)[CH2:4][OH:3])[CH3:27]

참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 22930682Ethyl 3-ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzoate

생성물 1

HCID 694273333-Ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl alcohol수율 92.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of ethyl-3-ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzoate (5.40 g) in tetrahydrofuran (80 ml) was gradually added aluminum lithium hydride (540 mg) at 0° C. and the mixture was stirred for 1 hr. Sodium sulfate 10 hydrate (4.60 g) was added to the reaction mixture and the mixture was further stirred for 30 min. The insoluble materials were filtered off, and the filtrate was concentrated. The obtained crystals were recrystallized from ethyl acetate-isopropyl ether to give 3-ethoxy-5-(5-methyl-2-phenyl-4-oxazolylmethoxy)benzyl alcohol (4.44 g, 92%) as colorless needle-shaped crystals. melting point: 103–104° C.

후처리

  1. customat 0° C.
  2. stirringthe mixture was further stirred for 30 min
  3. filtrationThe insoluble materials were filtered off
  4. concentrationthe filtrate was concentrated
  5. customThe obtained crystals were recrystallized from ethyl acetate-isopropyl ether

출처 및 근거

ORD 기록
ord-b2c65d1d1220496bb4a50abd327355f0
출처 데이터셋
uspto-grants-2007_07
특허 번호
US07241785B2

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