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Ammonium formate → 2(S)-amino-1-cyclohexyl-3(S)-hydroxy-6-methylheptane

HRID 259832
ノート
印刷プレビュー

反応式

HRID 259832 の反応式
C([N:8]([C@H:16]([C@@H:24]([OH:30])[CH2:25][CH2:26][CH:27]([CH3:29])[CH3:28])[CH2:17][CH:18]1[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1)CC1C=CC=CC=1)C1C=CC=CC=1.C([O-])=O.[NH4+]>CO.[C].[Pd]>[NH2:8][C@H:16]([C@@H:24]([OH:30])[CH2:25][CH2:26][CH:27]([CH3:28])[CH3:29])[CH2:17][CH:18]1[CH2:19][CH2:20][CH2:21][CH2:22][CH2:23]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 543040652(S)-(N,N-Dibenzylamino)-1-cyclohexyl-3(S)-hydroxy-6-methylheptane

生成物 1

HCID 146717222(S)-amino-1-cyclohexyl-3(S)-hydroxy-6-methylheptane収率 148.1%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 887Methanol溶媒

実験手順

2(S)-(N,N-Dibenzylamino)-1-cyclohexyl-3(S)-hydroxy-6-methylheptane (5 g) was dissolved in methanol (50 ml). Ammonium formate (6.18 g) and then 10% palladium-carbon (50% wet, 0.5 g) were added thereto, and the mixture was vigorously stirred at room temperature. After the completion of the reaction, the reaction mixture was filtered, and the filtrate was concentrated under reduced pressure. Ethyl acetate and water were added to the concentrated residue for extraction. The organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure to give 4.13 g of 2(S)-amino-1-cyclohexyl-3(S)-hydroxy-6-methylheptane.

後処理

  1. customAfter the completion of the reaction
  2. filtrationthe reaction mixture was filtered
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. additionEthyl acetate and water were added to the concentrated residue for extraction
  5. washThe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-fd8dddd55e1c422eb61b0cff155d2803
出典データセット
uspto-grants-1996_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05523410

反応ノート

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