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

HRID 2388693
ノート
印刷プレビュー

反応式

HRID 2388693 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a9e22ff8c5194fc8972603269962041e
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08268814B2

反応ノート

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