Water → 1-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acid

HRID 50052

반응식

HRID 50052 반응식
C(N(CC)CC)C.O.[NH:9]1[CH2:17][CH2:16][CH:12]([C:13]([OH:15])=[O:14])[CH2:11][CH2:10]1.[C:18](=O)([O:24]C(C)(C)C)[O:19][C:20]([CH3:23])([CH3:22])[CH3:21]>O1CCOCC1>[C:20]([O:19][C:18]([N:9]1[CH2:17][CH2:16][CH:12]([C:13]([OH:15])=[O:14])[CH2:11][CH2:10]1)=[O:24])([CH3:23])([CH3:22])[CH3:21]

참가 물질

6

반응물 4

HCID 962WaterHCID 37734-Piperidinecarboxylic acidHCID 8471TriethylamineHCID 10219638Carbonic acid, bis(1,1-dimethylethyl) ester

생성물 1

HCID 3928711-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acid수율 95.8%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
60 °C

실험 절차

8.6 g of triethylamine and 20 ml of water are added to a solution of 10 g of isonipecotic acid in 100 ml of dioxane and the mixture is heated to 60° C. 20.25 g of di-tert-butyl carbonate are then added dropwise and the mixture is stirred for 1 hour at 60° C. and refluxed for 30 minutes. It is concentrated under vacuum, the residue is taken up with water and acidified to pH 3 by the addition of 2 N HCl solution and the precipitate formed is filtered off to give 17 g of the expected product.

후처리

  1. temperaturerefluxed for 30 minutes
  2. concentrationIt is concentrated under vacuum
  3. additionacidified to pH 3 by the addition of 2 N HCl solution
  4. customthe precipitate formed
  5. filtrationis filtered off

출처 및 근거

ORD 기록
ord-2839b4b8535f4f1284e5c5ef0171095d
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06710042B2

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