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1-Chloro-4-(chloromethyl)benzene → Ethyl-3-(4-chlorobenzyl)-N-Boc-piperidin-3-caroxylate

HRID 2259926
ノート
印刷プレビュー

反応式

HRID 2259926 の反応式
[CH2:1]([O:3][C:4](=[O:18])[CH:5]1[CH2:10][CH2:9][CH2:8][N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:6]1)[CH3:2].C[Si]([N-][Si](C)(C)C)(C)C.[Li+].[Cl:29][C:30]1[CH:37]=[CH:36][C:33]([CH2:34]Cl)=[CH:32][CH:31]=1.C(=O)(O)[O-].[Na+]>O1CCCC1>[CH2:1]([O:3][C:4]([C:5]1([CH2:34][C:33]2[CH:36]=[CH:37][C:30]([Cl:29])=[CH:31][CH:32]=2)[CH2:10][CH2:9][CH2:8][N:7]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:6]1)=[O:18])[CH3:2]
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 77231-Chloro-4-(chloromethyl)benzeneHCID 3577271-Tert-butyl 3-ethyl piperidine-1,3-dicarboxylateHCID 516892Sodium BicarbonateHCID 2733832Lithium hexamethyldisilazane

生成物 1

HCID 19962177Ethyl-3-(4-chlorobenzyl)-N-Boc-piperidin-3-caroxylate

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒
2 回

実験手順

A solution of ethyl-N-boc-nipecotate (45 g, 0.18 mole) in tetrahydrofuran (200 mL) at -40° C. was treated with a solution of lithium bis (trimethylsilyl)amide in tetrahydrofuran (320 mL of a 1M solution). The solution was stirred at -40° for 15 minutes at which time 4-Chlorobenzyl chloride (34.59 g, 0.215 moles) was added and the reaction warmed to room temperature over 1.5 hours. The reaction was poured into saturated aqueous sodium bicarbonate (1 L) and extracted with ethyl acetate (3×500 mL). The combined organic extracts were dried over anhydrous magnesium sulfate, filtered, and concentrated at reduced pressure. The residue was chromatographed on silica gel with 30% ethyl acetate/hexane as eluent to give 36.5 g.

後処理

  1. additionwas added
  2. extractionextracted with ethyl acetate (3×500 mL)
  3. dry with materialThe combined organic extracts were dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated at reduced pressure
  6. customThe residue was chromatographed on silica gel with 30% ethyl acetate/hexane as eluent
  7. customto give 36.5 g

出典と根拠

ORDレコード
ord-705351222da34a7fab91f46ec8ed53c7
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05475109

反応ノート

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