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Sodium Carbonate → HCID 58574225、化合物

HRID 1619430
ノート
印刷プレビュー

反応式

HRID 1619430 の反応式
O=[C:2]1[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[C:10]([O:12]CC)=O.[NH2:15][C:16]1[CH:17]=[C:18]([CH:23]=[CH:24][N:25]=1)[C:19]([O:21][CH3:22])=[O:20].C(=O)([O-])[O-].[Na+].[Na+]>ClCCCl>[CH3:22][O:21][C:19]([C:18]1[CH:23]=[CH:24][N:25]2[C:10](=[O:12])[C:3]3[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][C:2]=3[N:15]=[C:16]2[CH:17]=1)=[O:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 227421Ethyl 2-oxocyclooctane-1-carboxylateHCID 236984Methyl 2-aminopyridine-4-carboxylate

生成物 1

HCID 58574225HCID 58574225、化合物収率 10.9%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A solution of ethyl 2-oxocyclooctanecarboxylate (1 g, 5.05 mmol) and methyl 2-aminoisonicotinate (0.768 g, 5.05 mmol) in PPA (2.5 mL) and 1,2-dichloroethane (5 mL) was stirred at 85° C. for 18 hours. The reaction mixture was then cooled to ambient temperature. A chilled saturated sodium carbonate solution was added to adjust pH to 8. The resulting mixture was extracted with ethyl acetate (4×100 mL). The combined organic layers were washed with brine and dried over anhydrous sodium sulfate. After filtration and concentration, the crude product was purified by silica gel chromatography purification to afford 157 mg of desired product.

後処理

  1. extractionThe resulting mixture was extracted with ethyl acetate (4×100 mL)
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationAfter filtration and concentration
  5. customthe crude product was purified by silica gel chromatography purification

出典と根拠

ORDレコード
ord-1f23e14733cf4faf95513b1b009ab46e
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08772301B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート