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Chlorobenzene → N-[3,5-Bis(trifluoromethyl)phenyl]-5-chloro-2-hydroxy-N-methylbenzamide

HRID 2384319
ノート
印刷プレビュー

反応式

HRID 2384319 の反応式
[Cl:1][C:2]1[CH:10]=[C:6]([C:7]([OH:9])=O)[C:5]([OH:11])=[CH:4][CH:3]=1.[F:12][C:13]([F:27])([F:26])[C:14]1[CH:15]=[C:16]([CH:19]=[C:20]([C:22]([F:25])([F:24])[F:23])[CH:21]=1)[NH:17][CH3:18].P(Cl)(Cl)Cl.ClC1C=CC=CC=1>CCCCCC>[F:12][C:13]([F:26])([F:27])[C:14]1[CH:15]=[C:16]([N:17]([CH3:18])[C:7](=[O:9])[C:6]2[CH:10]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[OH:11])[CH:19]=[C:20]([C:22]([F:23])([F:25])[F:24])[CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 7964ChlorobenzeneHCID 94475-Chlorosalicylic AcidHCID 24387Phosphorus trichlorideHCID 13803020N-Methyl-3,5-bis(trifluoromethyl)aniline

生成物 1

HCID 10318656N-[3,5-Bis(trifluoromethyl)phenyl]-5-chloro-2-hydroxy-N-methylbenzamide収率 18.9%

試薬・触媒・溶媒 1

HCID 8058
Hexane
溶媒

実験手順

A mixture of 5-chlorosalicylic acid (173 mg, 1 mmol), 3,5-bis(trifluoromethyl)-N-methylaniline (243 mg, 1 mmol), phosphorus trichloride (44 μl, 0.5 mmol) and monochlorobenzene (5 mL) was refluxed for 3 hours under argon atmosphere. After the reaction mixture was cooled to room temperature, n-hexane (50 mL) was added, and the separated crude crystal was filtered and dissolved in ethyl acetate (50 mL). After the ethyl acetate solution was washed with water and brine one after another, dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (n-hexane:ethyl acetate=2:1) to give the title compound (75 mg, 18.9%) as a white crystal.

後処理

  1. temperaturewas refluxed for 3 hours under argon atmosphere
  2. customthe separated crude crystal
  3. filtrationwas filtered
  4. dissolutiondissolved in ethyl acetate (50 mL)
  5. washAfter the ethyl acetate solution was washed with water and brine one after another,
  6. dry with materialdried over anhydrous sodium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe obtained residue was purified by column chromatography on silica gel (n-hexane:ethyl acetate=2:1)

出典と根拠

ORDレコード
ord-5326c11ab33e482f93fdda82cac62fed
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08263657B2

反応ノート

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