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Piperidine → HCID 68546659, 화합물

HRID 1841881
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HRID 1841881 반응식
[C:1]([CH2:3][C:4]([NH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[O:5])#[N:2].[CH3:15][N:16]([CH3:27])[C:17]1[CH:18]=[C:19]([CH:22]=[CH:23][C:24]=1[O:25][CH3:26])[CH:20]=O.N1CCCCC1>N1C=CC=CC=1>[C:1]([C:3](=[CH:20][C:19]1[CH:22]=[CH:23][C:24]([O:25][CH3:26])=[C:17]([N:16]([CH3:27])[CH3:15])[CH:18]=1)[C:4]([NH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[O:5])#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8082PiperidineHCID 12225606Benzaldehyde, 3-(dimethylamino)-4-methoxy-HCID 85875172HCID 85875172, 화합물

생성물 1

HCID 68546659HCID 68546659, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

3.96 g (20 mMol 6-(2-cyan-acetylamino)hexanoic acid was dissolved in 27 ml pyridine. 3.64 g (20 mMol) 3-dimethylamino-4-methoxybenzaldehyde and 0.6 mL piperidine were added to the solution and the reaction mixture was stirred for 20 hours. After evaporation of the reaction mixture the residue was solved in 150 ml ethyl acetate and 150 ml water and the pH was adjusted with pure acetic acid to 4.2. The aqueous phase was extracted with ethyl acetate. The collected ethyl acetate phases were washed with NaCl-Solution, dried and evaporated. The residue was chromatographed on SiO2 with ethyl acetate under low pressure. The product was crystallized from little ethyl acetate.

후처리

  1. customAfter evaporation of the reaction mixture the residue
  2. extractionThe aqueous phase was extracted with ethyl acetate
  3. washThe collected ethyl acetate phases were washed with NaCl-Solution
  4. customdried
  5. customevaporated
  6. customThe residue was chromatographed on SiO2 with ethyl acetate under low pressure
  7. customThe product was crystallized from little ethyl acetate

출처 및 근거

ORD 기록
ord-11b227e362d247d6abe34ac0f6d8f0d4
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946129B2

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