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

HRID 1640094ノート

反応式

HRID 1640094 の反応式
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]

参加物

5

反応物 2

HCID 120027444-(3,5-Bis-trifluoromethyl-benzyl)-2-methylanilineHCID 57450847HCID 57450847、化合物

生成物 1

HCID 6956Phthalamide収率 92.3%

試薬・触媒・溶媒 2

HCID 521998p-Toluenesulfonic acid monohydrate触媒HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-60c32869c3ba4c569d311b7cd3b80996
出典データセット
uspto-grants-2012_02
特許番号
US08110689B2

反応ノート

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