Dimethylformamide → N,N-dimethyl-4-phenylpiperidine-4-carboxamide

HRID 1739110

반응식

HRID 1739110 반응식
C([N:3]([CH2:6][CH3:7])[CH2:4][CH3:5])C.Cl.[CH3:9]NC.F[P-](F)(F)(F)(F)F.N1(O[P+](N(C)C)(N(C)C)N(C)C)[C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=2N=N1.[CH3:39][N:40]([CH:42]=[O:43])[CH3:41]>C(Cl)Cl>[CH3:39][N:40]([CH3:41])[C:42]([C:9]1([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH2:5][CH2:4][NH:3][CH2:6][CH2:7]1)=[O:43]

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 10473Dimethylamine, hydrochlorideHCID 151348Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate

생성물 1

HCID 417393N,N-dimethyl-4-phenylpiperidine-4-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

8.1 g of triethylamine and then 4.9 g of dimethylamine hydrochloride are added to a solution of 6.11 g of the compound obtained in step A of PREPARATION 1.21 in 20 ml of DCM and 20 ml of DMF. The mixture is cooled in an ice bath, 9.73 g of BOP are added and the mixture is left stirring for 3 hours while allowing the temperature to rise to RT. The mixture is concentrated under vacuum, the residue is extracted with ether, the organic phase is washed with water, with a pH 2 buffer solution, with 10% NaOH solution, with water and with saturated NaCl solution and dried over MgSO4 and the solvent is evaporated off under vacuum. 6.45 g of the expected product are obtained.

후처리

  1. temperatureThe mixture is cooled in an ice bath
  2. waitthe mixture is left
  3. customto rise to RT
  4. concentrationThe mixture is concentrated under vacuum
  5. extractionthe residue is extracted with ether
  6. washthe organic phase is washed with water, with a pH 2 buffer solution, with 10% NaOH solution, with water and with saturated NaCl solution
  7. dry with materialdried over MgSO4
  8. customthe solvent is evaporated off under vacuum

출처 및 근거

ORD 기록
ord-66f1efa0e0d8446c8561ed97495564ec
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05965580

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