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Ammonium formate → (S)-3-Methyl-3-[2-(tetrahydropyran-2-yloxy)ethoxymethyl]piperidine

HRID 2407315
ノート
印刷プレビュー

反応式

HRID 2407315 の反応式
C([N:8]1[CH2:13][CH2:12][CH2:11][C@:10]([CH3:25])([CH2:14][O:15][CH2:16][CH2:17][O:18][CH:19]2[CH2:24][CH2:23][CH2:22][CH2:21][O:20]2)[CH2:9]1)C1C=CC=CC=1.C([O-])=O.[NH4+]>CO.[Pd]>[CH3:25][C@:10]1([CH2:14][O:15][CH2:16][CH2:17][O:18][CH:19]2[CH2:24][CH2:23][CH2:22][CH2:21][O:20]2)[CH2:11][CH2:12][CH2:13][NH:8][CH2:9]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 2

HCID 2723923Ammonium formateHCID 66727401(S)-1-Benzyl-3-methyl-3-[2-(tetrahydropyran-2-yloxy)ethoxymethyl]piperidine

生成物 1

HCID 66727215(S)-3-Methyl-3-[2-(tetrahydropyran-2-yloxy)ethoxymethyl]piperidine収率 83.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒2 回

実験手順

(S)-1-Benzyl-3-methyl-3-[2-(tetrahydropyran-2-yloxy)ethoxymethyl]piperidine (1.14 g, 3.3 mmol) in MeOH (11 ml) was added to a suspension of Pd/C (0.23 g) in MeOH (11 ml), followed by ammonium formate (1.03 g, 16.4 mmol). The mixture was refluxed for 2 h, after which it was cooled and filtered through Celite. The catalyst was washed with DCM and the combined organic phases were evaporated to dryness. To the residue was added brine (15 ml) and the solution was extracted with EtOAc (3×30 ml). The extracts were combined, dried, filtered and evaporated to yield 0.71 g of the debenzylated product.

後処理

  1. temperatureThe mixture was refluxed for 2 h
  2. temperatureafter which it was cooled
  3. filtrationfiltered through Celite
  4. washThe catalyst was washed with DCM
  5. customthe combined organic phases were evaporated to dryness
  6. additionTo the residue was added brine (15 ml)
  7. extractionthe solution was extracted with EtOAc (3×30 ml)
  8. customdried
  9. filtrationfiltered
  10. customevaporated

出典と根拠

ORDレコード
ord-5eda3c4add934034837177a7c9dda0a9
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08809536B2

反応ノート

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