7,8-Dihydro-2-(phenylmethoxy)-5(6H)-quinolinone → HCID 10061627、化合物

HRID 1195157ノート

反応式

HRID 1195157 の反応式
[CH3:1][Mg]Br.[O:4]=[C:5]1[CH2:14][CH2:13][CH2:12][C:11]2[N:10]=[C:9]([O:15][CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH:8]=[CH:7][C:6]1=2>C1(C)C=CC=CC=1>[OH:4][C:5]1([CH3:1])[CH2:14][CH2:13][CH2:12][C:11]2[N:10]=[C:9]([O:15][CH2:16][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[CH:8]=[CH:7][C:6]1=2

参加物

4

反応物 2

HCID 104449777,8-Dihydro-2-(phenylmethoxy)-5(6H)-quinolinoneHCID 178418573HCID 178418573、化合物

生成物 1

HCID 10061627HCID 10061627、化合物収率 92%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Methylmagnesium bromide (3.0M in diethyl ether, 47 ml) was added dropwise to a solution of 5,6,7,8-tetrahydro-5-oxo-2-(phenylmethoxy)quinoline (29.6 g) and toluene (1l) at 0° C. The reaction mixture was allowed to warm to room temperature, with stirring. The reaction mixture was then quenched with saturated ammonium chloride solution, the layers were separated, and the aqueous phase was extracted with ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated to provide 31.7 g (92.0%) of product.

後処理

  1. customThe reaction mixture was then quenched with saturated ammonium chloride solution
  2. customthe layers were separated
  3. extractionthe aqueous phase was extracted with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-99c18dc6a5b34c158cfbf78a21b85efd
出典データセット
uspto-grants-1992_05
特許番号
US05110815

反応ノート

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