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

HRID 1739110

反応式

HRID 1739110 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-66f1efa0e0d8446c8561ed97495564ec
出典データセット
uspto-grants-1999_10
特許番号
US05965580

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