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HCID 67969353、化合物 → tert-Butyl ((3S,5R)-5-methylpiperidin-3-yl)carbamate

HRID 1499488
ノート
印刷プレビュー

反応式

HRID 1499488 の反応式
C([N:8]1[CH2:13][C@H:12]([CH3:14])[CH2:11][C@H:10]([NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])[CH2:9]1)C1C=CC=CC=1>CO.[Pd]>[CH3:14][C@H:12]1[CH2:13][NH:8][CH2:9][C@@H:10]([NH:15][C:16](=[O:22])[O:17][C:18]([CH3:21])([CH3:20])[CH3:19])[CH2:11]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 67969353HCID 67969353、化合物

生成物 1

HCID 57433105tert-Butyl ((3S,5R)-5-methylpiperidin-3-yl)carbamate

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

10 wt % Pd on carbon (120 mg, 0.11 mmol) was added to a solution of tert-butyl [(3S,5R)-1-benzyl-5-methylpiperidin-3-yl]carbamate (0.34 g, 1.1 mmol) in MeOH (15.0 mL). The mixture was stirred at room temperature under a hydrogen atmosphere (1 atm.) for 15 h. The reaction was filtered through a pad of diatomaceous earth (eluted with MeOH), and then concentrated under reduced pressure. The resulting crude product was used directly in the next step residue without further purification (0.21 g, 88%). LCMS calc. for C11H23N2O2 (M+H)+: m/z=215.2. found 215.2. 1H NMR (CDCl3, 400 MHz) δ 4.33 (1H, m), 3.46 (1H, m), 3.25 (1H, m), 2.94 (1H, dd, J=3.6 and 12.8 Hz), 2.18-2.02 (3H, m), 1.60 (1H, m), 1.43 (9H, s), 0.85 (3H, d, J=6.8 Hz) ppm.

後処理

  1. filtrationThe reaction was filtered through a pad of diatomaceous earth (eluted with MeOH)
  2. concentrationconcentrated under reduced pressure
  3. customThe resulting crude product was used directly in the next step residue without further purification (0.21 g, 88%)

出典と根拠

ORDレコード
ord-c5172ba018aa497fb8871377b2221405
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09200004B2

反応ノート

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