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

HRID 1585739

反応式

HRID 1585739 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-9047e44273714032bda06a9a8e37f925
出典データセット
uspto-grants-1999_08
特許番号
US05939411

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