Water → (S)-1-Benzyl-3-methylpiperidine-3-carboxylic acid ethyl ester

HRID 453817노트

반응식

HRID 453817 반응식
[CH2:1]([O:3][C:4]([C@@:6]1([CH3:12])[CH2:11][CH2:10][CH2:9][NH:8][CH2:7]1)=[O:5])[CH3:2].[CH2:13](Cl)[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C>[CH2:1]([O:3][C:4]([C@@:6]1([CH3:12])[CH2:11][CH2:10][CH2:9][N:8]([CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:7]1)=[O:5])[CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 7503Benzyl ChlorideHCID 11430Potassium CarbonateHCID 23389262(S)-Ethyl 3-methylpiperidine-3-carboxylate

생성물 1

HCID 66727374(S)-1-Benzyl-3-methylpiperidine-3-carboxylic acid ethyl ester수율 92.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

(S)-3-Methylpiperidine-3-carboxylic acid ethyl ester (1.16 g, 6.8 mmol), benzyl chloride (0.82 ml, 7.1 mmol), K2CO3 (1.22 g, 8.8 mmol) and KI (0.056 g) were stirred and heated in DMF (50 ml) for 2.5 h. The cooled solution was poured into water and extracted with EtOAc (3×50 ml). The combined extracts were washed several times with water and finally with brine. Drying, filtering and evaporation of the solvent gave 1.64 g of the target compound as a yellowish oil.

후처리

  1. extractionextracted with EtOAc (3×50 ml)
  2. washThe combined extracts were washed several times with water
  3. customDrying
  4. filtrationfiltering
  5. customevaporation of the solvent

출처 및 근거

ORD 기록
ord-2639e903afd74fff95cc9f08388df4c2
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08492549B2

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