4-(3,5-Bis-trifluoromethyl-benzyl)-2-methylaniline → Phthalamide

HRID 1640094노트

반응식

HRID 1640094 반응식
Cl[C:2]1[CH:10]=[CH:9][CH:8]=[C:7]2[C:3]=1[C:4](=[N:12][C@@H](C)CSC)[O:5][C:6]2=[O:11].FC(F)(F)C1C=C(C=C(C(F)(F)F)C=1)CC1C=CC([NH2:28])=C(C)C=1>C(#N)C.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>[C:6]([NH2:28])(=[O:11])[C:7]1[C:3](=[CH:2][CH:10]=[CH:9][CH:8]=1)[C:4]([NH2:12])=[O:5]

참가 물질

5

반응물 2

HCID 120027444-(3,5-Bis-trifluoromethyl-benzyl)-2-methylanilineHCID 57450847HCID 57450847, 화합물

생성물 1

HCID 6956Phthalamide수율 92.3%

시약·촉매·용매 2

HCID 521998p-Toluenesulfonic acid monohydrate촉매HCID 6342Acetonitrile용매

실험 절차

4-Chloro-3-[(S)-1-methyl-2-methylthioethylimino]-3-H-isobenzofuran-1-one (0.2 g) and 4-(3,5-bis-trifluoromethyl-benzyl)-2-methylaniline (0.22 g) were dissolved in acetonitrile (10 ml), to which p-toluenesulfonic acid hydrate (0.01 g) was added, and then stirred at room temperature for three hours. After the reaction, the solvent was distilled off under reduced pressure and the resultant residue was purified by silica gel column chromatography to obtain N1-[4-(3,5-bis-trifluoromethyl-benzyl)-2-methylphenyl]-3-chloro-N2-(S)-1-methyl-2-methylthioethyl)phthalamide (0.10 g).

후처리

  1. additionwas added
  2. customAfter the reaction
  3. distillationthe solvent was distilled off under reduced pressure
  4. customthe resultant residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-60c32869c3ba4c569d311b7cd3b80996
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110689B2

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