Water → N-(2,3-dichloro-4-hydroxyphenyl)-3-chloro-2,2-dimethylpropane-carboxamide

HRID 583223ノート

反応式

HRID 583223 の反応式
Cl[CH2:2][C:3]([CH3:8])([CH3:7])[C:4]([Cl:6])=O.[NH2:9][C:10]1[CH:15]=[CH:14][C:13]([OH:16])=[C:12]([Cl:17])[C:11]=1[Cl:18].O.[O:20]1CCC[CH2:21]1>>[Cl:18][C:11]1[C:12]([Cl:17])=[C:13]([OH:16])[CH:14]=[CH:15][C:10]=1[NH:9][C:21]([CH2:2][C:3]([CH3:8])([CH3:7])[CH2:4][Cl:6])=[O:20]

参加物

5

反応物 4

HCID 962WaterHCID 8028TetrahydrofuranHCID 613453-Chloro-2,2-dimethylpropanoyl chlorideHCID 98775294-Amino-2,3-dichlorophenol

生成物 1

HCID 21311020N-(2,3-dichloro-4-hydroxyphenyl)-3-chloro-2,2-dimethylpropane-carboxamide

実験手順

1.55 g (0.01 mol) of chloropivaloyl chloride were added dropwise at 0° C. to a solution of 1.93 g (0.011 mol) of 4-amino-2,3-dichlorophenol in 30 ml of tetrahydrofuran, and stirring of the mixture was continued at 25° C. until starting compound was no longer detectable by thin-layer chromatography. The reaction mixture was subsequently poured into water and extracted three times using 20 ml of methylene chloride. The combined organic phases were washed twice using water, dried and concentrated. The residue was chroamtographed on silica gel (eluent: cyclohexane: ethyl acetate=2:1; yield: 0.75 g, m.p. 115° C.).

後処理

  1. customwas continued at 25° C.
  2. extractionextracted three times
  3. washThe combined organic phases were washed twice using water
  4. customdried
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-e7f1a394f6f94d4cb2c89623189c4d6e
出典データセット
uspto-grants-1999_07
特許番号
US05929119

反応ノート

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