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Benzyl Bromide → HCID 11322245、化合物

HRID 538670
ノート
印刷プレビュー

反応式

HRID 538670 の反応式
Cl.[NH:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][CH2:9][CH2:10][OH:11].C([O-])([O-])=O.[K+].[K+].[CH2:18](Br)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C(O)C>[CH2:18]([N:2]1[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:8][CH2:9][CH2:10][OH:11])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 201565333-(2-Piperidyl)-1-propanol Hydrochloride

生成物 1

HCID 11322245HCID 11322245、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution of compound 21 (3 g, 16.71 mmol) in ethanol (23 mL) was added K2CO3 (11.5 g, 83.55 mmol) portion-wise at ice cold conditions. Benzyl bromide (2 mL, 16.71 mmol) was then added and the reaction mixture was heated at reflux for 2 hours. The reaction mixture was filtered, and washed with EtOAc. The filtrate was concentrated, the residue was dissolved in EtOAc, washed with saturated NaHCO3 solution and brine, dried over Na2SO4, filtered and concentrated. The crude material was purified by 230-400 silica gel column chromatography using 1-3% MeOH-DCM as eluent to yield compound 22.

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureat reflux for 2 hours
  3. filtrationThe reaction mixture was filtered
  4. washwashed with EtOAc
  5. concentrationThe filtrate was concentrated
  6. dissolutionthe residue was dissolved in EtOAc
  7. washwashed with saturated NaHCO3 solution and brine
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe crude material was purified by 230-400 silica gel column chromatography

出典と根拠

ORDレコード
ord-4983f2ca5e8641988249e25b0a505db5
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08865741B2

反応ノート

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