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Lithium Hydroxide → 5-(1,1-Dimethylethyl) 6,7-dihydroisoxazolo[4,5-c]pyridine-3,5(4H)-dicarboxylate

HRID 2388693
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HRID 2388693 반응식
[OH-].[Li+].[O:3]1[C:11]2[CH2:10][CH2:9][N:8]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:7][C:6]=2[C:5]([C:19]([O:21]CC)=[O:20])=[N:4]1>C(O)C>[C:15]([O:14][C:12]([N:8]1[CH2:9][CH2:10][C:11]2[O:3][N:4]=[C:5]([C:19]([OH:21])=[O:20])[C:6]=2[CH2:7]1)=[O:13])([CH3:18])([CH3:16])[CH3:17]
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참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 576186205-Tert-butyl 3-ethyl 4H,5H,6H,7H-[1,2]oxazolo[4,5-C]pyridine-3,5-dicarboxylate

생성물 1

HCID 576186225-(1,1-Dimethylethyl) 6,7-dihydroisoxazolo[4,5-c]pyridine-3,5(4H)-dicarboxylate

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

An aqueous lithium hydroxide solution (0.54 g, 12.88 mol in 12.8 ml) was added dropwise to a solution of 5-tert-butyl 3-ethyl 6,7-dihydroisoxazolo[4,5-c]pyridine-3,5(4H)-dicarboxylate (3.2 g, 10.73 mmol) in ethanol (48 ml) at 0° C. and the mixture was stirred at room temperature for 3 hours. The mixture was then concentrated in vacuo, the residue was acidified with 10% strength citric acid and the mixture was extracted three times with ethyl acetate. The combined organic phases were dried with Na2SO4, filtered and concentrated in vacuo. The crude product was employed directly in the next stage without further purification.

후처리

  1. concentrationThe mixture was then concentrated in vacuo
  2. extractionthe mixture was extracted three times with ethyl acetate
  3. dry with materialThe combined organic phases were dried with Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude product was employed directly in the next stage without further purification

출처 및 근거

ORD 기록
ord-a9e22ff8c5194fc8972603269962041e
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08268814B2

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