Water → HCID 66987744, 화합물

HRID 333421

반응식

HRID 333421 반응식
[CH:1]1([NH:4][CH:5]2[CH2:10][CH2:9][N:8]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:7][CH2:6]2)[CH2:3][CH2:2]1.C(N(CC)CC)C.[C:25](Cl)(=O)[CH2:26][CH3:27].[OH2:30]>C1COCC1>[CH:26]1([CH2:2][CH2:3][C:1]([NH:4][CH:5]2[CH2:6][CH2:7][N:8]([C:11]([O:13][C:14]([CH3:15])([CH3:16])[CH3:17])=[O:12])[CH2:9][CH2:10]2)=[O:30])[CH2:27][CH2:25]1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 62324Propionyl chlorideHCID 2769591tert-Butyl 4-(cyclopropylamino)piperidine-1-carboxylate

생성물 1

HCID 66987744HCID 66987744, 화합물수율 89%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

0.8 g (3.3 mmol) of tert-butyl 4-cyclopropylaminopiperidine-1-carboxylate, 0.48 mL (3.3 mmol) of triethylamine and 0.56 mL (3.3 mmol) of propionyl chloride are dissolved in 50 mL of THF. The reaction medium is stirred for 2 hours at room temperature. The reaction is stopped by adding water and the organic products are then extracted with dichloromethane. The organic phase is dried and then evaporated. The crude product obtained is chromatographed on silica gel (eluent: 6/4 heptane/ethyl acetate). 0.87 g of tert-butyl 4-(cyclopropylpropionylamino)piperidine-1-carboxylate in the form of a colourless oil is obtained in a yield of 89%.

후처리

  1. extractionthe organic products are then extracted with dichloromethane
  2. customThe organic phase is dried
  3. customevaporated
  4. customThe crude product obtained
  5. customis chromatographed on silica gel (eluent: 6/4 heptane/ethyl acetate)

출처 및 근거

ORD 기록
ord-1de102abcc1d483ab3fa12abd58096c9
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877968B2

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