Water → N-[4-(4-Piperidinomethyl-2-pyridyloxy)-cis-2-butenyl]-2-chloroacetamide

HRID 52125

反応式

HRID 52125 の反応式
[N:1]1([CH2:7][C:8]2[CH:13]=[CH:12][N:11]=[C:10]([O:14][CH2:15]/[CH:16]=[CH:17]\[CH2:18][NH2:19])[CH:9]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[Cl:27][CH2:28][C:29](Cl)=[O:30].O>C(OCC)(=O)C>[N:1]1([CH2:7][C:8]2[CH:13]=[CH:12][N:11]=[C:10]([O:14][CH2:15]/[CH:16]=[CH:17]\[CH2:18][NH:19][C:29](=[O:30])[CH2:28][Cl:27])[CH:9]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 962WaterHCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 136724732-Buten-1-amine, 4-[[4-(1-piperidinylmethyl)-2-pyridinyl]oxy]-, (Z)-

生成物 1

HCID 67725626N-[4-(4-Piperidinomethyl-2-pyridyloxy)-cis-2-butenyl]-2-chloroacetamide収率 73%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

1.00 g of 4-(4-piperidinomethyl-2-pyridyloxy)-cis-2-butenylamine was dissolved in 20 ml of ethyl acetate. 0.54 ml of triethylamine was added to the solution, and the resulting mixture was cooled in an ice bath. 0.31 ml of 2-chloroacetyl chloride was added, and the mixture was stirred for 1 hour at room temperature. At the end of this time, water was added, and the reaction mixture was extracted with ethyl acetate. The extract was condensed by evaporation under reduced pressure, and the residue was purified by silica gel chromatography, eluted with a 1:19 by volume mixture of methanol and ethyl acetate, to give 0.94 g (yield 73%) of the title compound as an oil.

後処理

  1. temperaturethe resulting mixture was cooled in an ice bath
  2. extractionthe reaction mixture was extracted with ethyl acetate
  3. customcondensed
  4. customby evaporation under reduced pressure
  5. customthe residue was purified by silica gel chromatography
  6. washeluted with a 1:19 by volume mixture of methanol and ethyl acetate

出典と根拠

ORDレコード
ord-373d80380d2d45d0b2bb19c0f492ba9a
出典データセット
uspto-grants-1997_04
特許番号
US05616579

関連ノート

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