Ethanol → ethyl 2-[(3R)-piperidin-3-yl]acetate

HRID 1948489ノート

反応式

HRID 1948489 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][C@H:10]([CH2:14][C:15]([OH:17])=[O:16])[CH2:9]1)=O)(C)(C)C.[CH2:18](O)[CH3:19]>>[NH:8]1[CH2:13][CH2:12][CH2:11][C@H:10]([CH2:14][C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:9]1

参加物

3

反応物 2

HCID 702EthanolHCID 15020852-[(3R)-1-[(2-methylpropan-2-yl)oxycarbonyl]piperidin-3-yl]acetic acid

生成物 1

HCID 7161133ethyl 2-[(3R)-piperidin-3-yl]acetate

実験手順

To a mixture of (R)-2-(1-(tert-butoxycarbonyl)piperidin-3-yl)acetic acid (6 g, 24.66 mmol) in ethanol (20 mL) was bubbled HCl (g) for 10 minutes. The reaction mixture was stirred for 1 hr and then HCl was bubbled through the mixture for 5 minutes. After 1 hour, solvents were removed from the mixture in vacuo. The reaction mixture was diluted with ethyl acetate and washed with saturated NaHCO3. The aqueous layer was backextracted 2 times with 10% IPA/chloroform. The organic layers were combined, dried, and concentrated in vacuo to yield 4.05 g of (R)-ethyl 2-(piperidin-3-yl)acetate. MS (M+1)=172. HPLC Peak RT=0.96 minutes.

後処理

  1. customwas bubbled HCl (g) for 10 minutes
  2. customHCl was bubbled through the mixture for 5 minutes
  3. waitAfter 1 hour
  4. customsolvents were removed from the mixture in vacuo
  5. additionThe reaction mixture was diluted with ethyl acetate
  6. washwashed with saturated NaHCO3
  7. customdried
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-83251601302d47b59b2441b2409c8138
出典データセット
uspto-grants-2013_03
特許番号
US08399451B2

反応ノート

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