Potassium Carbonate → 4-(2-Piperidin-1-yl-ethoxy)-phenylamine

HRID 898524ノート

反応式

HRID 898524 の反応式
C(=O)([O-])[O-].[K+].[K+].[NH2:7][C:8]1[CH:13]=[CH:12][C:11]([OH:14])=[C:10](Cl)[CH:9]=1.Cl[CH2:17][CH2:18][N:19]1[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1>C(#N)C>[N:19]1([CH2:18][CH2:17][O:14][C:11]2[CH:12]=[CH:13][C:8]([NH2:7])=[CH:9][CH:10]=2)[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 748271-(2-Chloroethyl)piperidineHCID 775784-Amino-2-chlorophenol

生成物 1

HCID 30160254-(2-Piperidin-1-yl-ethoxy)-phenylamine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

15.4 g (111.00 mmol) of potassium carbonate was added to a solution of 4.0 g (27.86 mmol) of 4-amino-2-chlorophenol and 5.1 g (27.86 mmol) of 1-(2-chloro-ethyl)-piperidine in 50 mL acetonitrile and the mixture was stirred for 48 hours at RT. The solvent was evaporated off i. vac., the residue was combined with water and the aqueous phase was exhaustively extracted with EtOAc. The combined org. extracts were washed with water, dried over magnesium sulphate, evaporated down i. vac. and the residue was purified by column chromatography (silica gel, dichloromethane/MeOH/conc. aqueous ammonia 90:10:1).

後処理

  1. customThe solvent was evaporated off i
  2. extractionthe aqueous phase was exhaustively extracted with EtOAc
  3. washextracts were washed with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated down i
  6. customand the residue was purified by column chromatography (silica gel, dichloromethane/MeOH/conc. aqueous ammonia 90:10:1)

出典と根拠

ORDレコード
ord-9ff1f5c11f9f45ccbee9c2d8612370b8
出典データセット
uspto-grants-2008_04
特許番号
US07351719B2

反応ノート

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