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

HRID 1586980ノート

反応式

HRID 1586980 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 (1 l) at 0° C. The reaction mixture was allowed to warm to room temperature, with stirring. The redaction mixture was then quenched with saturated ammonium chloride solution, the layers were separate, 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 redaction mixture was then quenched with saturated ammonium chloride solution
  2. customthe layers were separate
  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-7df3cb4e04364ccea154849a04e2794c
出典データセット
uspto-grants-1993_06
特許番号
US05216164

反応ノート

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