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Ammonium formate → (3R,4R)-1-tert-butyl 3-ethyl 4-aminopiperidine-1,3-dicarboxylate

HRID 1593468
ノート
印刷プレビュー

反応式

HRID 1593468 の反応式
C1([C@H]([NH:9][C@@H:10]2[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][C@H:11]2[C:23]([O:25][CH2:26][CH3:27])=[O:24])C)C=CC=CC=1.C([O-])=O.[NH4+]>CO.[Pd]>[NH2:9][C@@H:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:17])[CH2:12][C@H:11]1[C:23]([O:25][CH2:26][CH3:27])=[O:24]
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 11080151(3R,4R)-1-tert-butyl 3-ethyl 4-((R)-1-phenylethylamino)-piperidine-1,3-dicarboxylate

生成物 1

HCID 58745614(3R,4R)-1-tert-butyl 3-ethyl 4-aminopiperidine-1,3-dicarboxylate収率 96.2%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of 252D (1.18 g, 3.13 mmol) in MeOH (31 mL) was treated with ammonium formate (1.58 g, 25.1 mmol) and 10% Pd/C. The reaction mixture was heated to reflux for 14 hours then cooled to room temperature. The resulting solid was removed by filtration and washed with MeOH. The filtrate was dried (Na2SO4) and concentrated under reduced pressure to give 0.82 g (yield: 96%) of Compound 252E as an oil.

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 14 hours
  3. customThe resulting solid was removed by filtration
  4. washwashed with MeOH
  5. dry with materialThe filtrate was dried (Na2SO4)
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-080a6bbcc21c46389f8dbc61b8d99ce3
出典データセット
uspto-grants-2007_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07297695B2

反応ノート

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