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

HRID 583223노트

반응식

HRID 583223 반응식
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]

참가 물질

5

반응물 4

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

생성물 1

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

실험 절차

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.).

후처리

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

출처 및 근거

ORD 기록
ord-e7f1a394f6f94d4cb2c89623189c4d6e
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05929119

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