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Acetic Acid → 4-(N-(2-methyl-3-phenyl-2-(E)-propenyl)aminomethyl)-1-(1-naphthylsulfonyl)piperidine

HRID 2110834
ノート
印刷プレビュー

反応式

HRID 2110834 の反応式
[NH2:1][CH2:2][CH:3]1[CH2:8][CH2:7][N:6]([S:9]([C:12]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[CH:14][CH:13]=2)(=[O:11])=[O:10])[CH2:5][CH2:4]1.[CH3:22]/[C:23](=[CH:26]\[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)/[CH:24]=O.C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)(O)[O-].[Na+]>CCCCCC.C(OCC)(=O)C.ClCCCl>[CH3:22]/[C:23](=[CH:26]\[C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)/[CH2:24][NH:1][CH2:2][CH:3]1[CH2:8][CH2:7][N:6]([S:9]([C:12]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[CH:14][CH:13]=2)(=[O:11])=[O:10])[CH2:5][CH2:4]1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 176Acetic Acid2 回HCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 5372813alpha-METHYLCINNAMALDEHYDEHCID 688620304-Aminomethyl-1-(1-naphthylsulfonyl)piperidine

生成物 1

HCID 688606314-(N-(2-methyl-3-phenyl-2-(E)-propenyl)aminomethyl)-1-(1-naphthylsulfonyl)piperidine
収率 86%

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒HCID 8058Hexane溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

A mixture of 4-aminomethyl-1-(1-naphthylsulfonyl)piperidine (intermediate in the preparation of the compound of Example 34, 450 mg, 1.5 mmol), (E)-2-methyl-3-phenylpropenal (438 mg, 3.0 mmol), acetic acid (240 mg, 4.0 mmol), and 1,2-dichloroethane (50 mL) was stirred under argon at room temperature for 3 h before sodium triacetoxyborohydride (1.27 g, 6.0 mmol) and more acetic acid (360 mg, 6.0 mmol) were added. After 16 h saturated aqueous sodium bicarbonate (50 mL) was added, and the aqueous and organic phases were separated. The aqueous phase was extracted with dichloromethane (50 mL twice), and the combined organic phases were dried (anhydrous sodium sulfate) and evaporated under vacuum. Column chromatography (silica gel, gradient of ethyl acetate in hexane rising to 100% ethyl acetate) provided 4-(N-(2-methyl-3-phenyl-2-(E)-propenyl)aminomethyl)-1-(1-naphthylsulfonyl)piperidine (561 mg, 86% yield) as an oil. TLC Rf=0.18, 100% ethyl acetate.

後処理

  1. additionwere added
  2. customthe aqueous and organic phases were separated
  3. extractionThe aqueous phase was extracted with dichloromethane (50 mL twice), and the combined organic phases
  4. dry with materialwere dried (anhydrous sodium sulfate)
  5. customevaporated under vacuum

出典と根拠

ORDレコード
ord-6996b9f5ac424b85ae41fb171e202bc7
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07517991B2

反応ノート

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