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Dimethylformamide → HCID 54112822、化合物

HRID 259240
ノート
印刷プレビュー

反応式

HRID 259240 の反応式
[CH2:1]1[O:13][C:12]2[CH:11]=[C:10]3[C:5]([C:6](=[O:22])[C:7]([C:19]([OH:21])=[O:20])=[CH:8][N:9]3[CH2:14][C:15]([F:18])([F:17])[F:16])=[CH:4][C:3]=2[O:2]1.CN(C)C=O.[CH3:28][C:29]([CH3:36])([CH3:35])[C:30]([O:32][CH2:33]Cl)=[O:31]>C(N(CC)CC)C>[CH2:1]1[O:13][C:12]2[CH:11]=[C:10]3[C:5]([C:6](=[O:22])[C:7]([C:19]([O:21][CH2:33][O:32][C:30](=[O:31])[C:29]([CH3:36])([CH3:35])[CH3:28])=[O:20])=[CH:8][N:9]3[CH2:14][C:15]([F:18])([F:17])[F:16])=[CH:4][C:3]=2[O:2]1
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 6228DimethylformamideHCID 87885Chloromethyl pivalateHCID 20356988HCID 20356988、化合物

生成物 1

HCID 54112822HCID 54112822、化合物

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

To a mixture of 2.6 g. 6,7-methylenedioxy-1-(2,2,2-trifluoroethyl)-4(1H)-quinolone-3-carboxylic acid and 35 ml. of dimethyl formamide was added 1.4 g. of triethylamine. The mixture was warmed to 55° and kept there for 1/2 hour. 2.8 g. of chloromethyl trimethylacetate was then added and the resulting mixture was stirred at 55° for 5 hours. The cooled solution was diluted with 150 ml. of ethyl acetate and washed with water. The ethyl acetate solution was dried over magnesium sulfate and concentrated. The solid residue, 6,7-methylenedioxy-1-(2,2,2-trifluoroethyl)-4(1H)-quinolone-3-carboxylic acid, trimethylacetoxymethyl ester, was recrystallized from CH2Cl2 -ether mixture; m.p. 190°-1°.

後処理

  1. additionTo a mixture of 2.6 g
  2. temperatureThe mixture was warmed to 55°
  3. additionThe cooled solution was diluted with 150 ml
  4. washof ethyl acetate and washed with water
  5. dry with materialThe ethyl acetate solution was dried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe solid residue, 6,7-methylenedioxy-1-(2,2,2-trifluoroethyl)-4(1H)-quinolone-3-carboxylic acid, trimethylacetoxymethyl ester, was recrystallized from CH2Cl2 -ether mixture

出典と根拠

ORDレコード
ord-cb4dda06b037417f9dedbedae2aefec4
出典データセット
uspto-grants-1977_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04036962

反応ノート

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