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Benzaldehyde → 1-{[(3S)-1-Benzylpiperidin-3-yl]methyl}-N-(3,4-dichlorophenyl)piperidine-4-carboxamide

HRID 603236
ノート
印刷プレビュー

反応式

HRID 603236 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]([CH:12]2[CH2:17][CH2:16][N:15]([CH2:18][C@@H:19]3[CH2:24][CH2:23][CH2:22][NH:21][CH2:20]3)[CH2:14][CH2:13]2)=[O:11])[CH:5]=[CH:6][C:7]=1[Cl:8].[CH:25](=O)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClCCl>[CH2:25]([N:21]1[CH2:22][CH2:23][CH2:24][C@@H:19]([CH2:18][N:15]2[CH2:14][CH2:13][CH:12]([C:10]([NH:9][C:4]3[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=3)=[O:11])[CH2:17][CH2:16]2)[CH2:20]1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=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 240BenzaldehydeHCID 5049666Sodium triacetoxyborohydride2 回HCID 57656947N-(3,4-dichlorophenyl)-1-[(3R)-piperidin-3-ylmethyl]piperidine-4-carboxamide

生成物 1

HCID 117195521-{[(3S)-1-Benzylpiperidin-3-yl]methyl}-N-(3,4-dichlorophenyl)piperidine-4-carboxamide収率 15%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a mixture of N-(3,4-dichlorophenyl)-1-[(3R)-piperidin-3-ylmethyl]piperidine-4-carboxamide (150 mg) and benzaldehyde (0.04 mL) in dichloromethane was added sodium triacetoxyborohydride (103 mg). The reaction mixture was stirred at room temperature for 18 hours. The reaction was incomplete so sodium triacetoxyborohydride (50 mg) was added and the mixture was stirred for 48 hours. The reaction mixture was partitioned between dichloromethane and water and the organic layer was washed with brine. The organic extract was dried over magnesium sulfate and evaporated. The residue was purified by silica column chromatography, eluting with a gradient of 0 to 10% MeOH in dichloromethane to give the title compound as a white solid (28 mg, 15%)

後処理

  1. additionwas added
  2. stirringthe mixture was stirred for 48 hours
  3. customThe reaction mixture was partitioned between dichloromethane and water
  4. washthe organic layer was washed with brine
  5. extractionThe organic extract
  6. dry with materialwas dried over magnesium sulfate
  7. customevaporated
  8. customThe residue was purified by silica column chromatography
  9. washeluting with a gradient of 0 to 10% MeOH in dichloromethane

出典と根拠

ORDレコード
ord-88956684dc1542d7b17e1cd4978f07ef
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07906645B2

反応ノート

読み込み中…

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