Tert-Butylamine → 2-(4-Amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanol

HRID 11899

反応式

HRID 11899 の反応式
[NH2:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5]([CH:12]2[O:14][CH2:13]2)=[CH:4][C:3]=1[Cl:15].[C:16]([NH2:20])([CH3:19])([CH3:18])[CH3:17]>C(O)C>[NH2:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5]([CH:12]([NH:20][C:16]([CH3:19])([CH3:18])[CH3:17])[CH2:13][OH:14])=[CH:4][C:3]=1[Cl:15]

参加物

4

反応物 2

HCID 6385Tert-ButylamineHCID 15067147(4-Amino-3-chloro-5-trifluoromethyl-phenyl)-ethylene oxide

生成物 1

HCID 99977892-(4-Amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanol収率 20%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

5.2 g (0.022 mol) of (4-amino-3-chloro-5-trifluoromethyl-phenyl)-ethylene oxide was dissolved in 26 ml of anhydrous ethanol and treated with 5.1 ml (0.049 mol) of tert-butylamine. The mixture was refluxed for 13 h, and then evaporated. The residue was extracted with 2N hydrochloric acid for several times. Aqueous layers were combined and extracted with toluene and treated with activated carbon. The pH was adjusted to 10 with 20% sodium hydroxide solution. The precipitate was collected by filtration, 2-(4-amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanol was obtained. Yield 20–30%; melting point 85–90° C.

後処理

  1. temperatureThe mixture was refluxed for 13 h
  2. customevaporated
  3. extractionThe residue was extracted with 2N hydrochloric acid for several times
  4. extractionextracted with toluene
  5. additiontreated with activated carbon
  6. filtrationThe precipitate was collected by filtration

出典と根拠

ORDレコード
ord-5946892308ac4131bb6fd116f5fb02cd
出典データセット
uspto-grants-2006_08
特許番号
US07098364B2

関連ノート

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