4-Iodobenzoyl chloride → (4-Dimethylamino-piperidin-1-yl)-(4-iodo-phenyl)-methanone

HRID 529768노트

반응식

HRID 529768 반응식
[I:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[CH:4][CH:3]=1.[CH3:11][N:12]([CH3:19])[CH:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1>C(Cl)Cl.C([O-])([O-])=O.[Na+].[Na+]>[CH3:11][N:12]([CH3:19])[CH:13]1[CH2:18][CH2:17][N:16]([C:6]([C:5]2[CH:9]=[CH:10][C:2]([I:1])=[CH:3][CH:4]=2)=[O:7])[CH2:15][CH2:14]1

참가 물질

5

반응물 2

HCID 743734-Iodobenzoyl chlorideHCID 417391N,N-Dimethylpiperidin-4-amine

생성물 1

HCID 60763941(4-Dimethylamino-piperidin-1-yl)-(4-iodo-phenyl)-methanone수율 98%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 10340Sodium Carbonate용매

실험 절차

A solution of 4-iodo-benzoyl chloride (4.72 g, 17.71 mmol) in DCM (70 mL) at 0° C. was treated with dimethyl-piperidin-4-yl-amine (2.27 g, 17.71 mmol). The resultant suspension was warmed to room temperature and stirred for 2.5 hours. The reaction mixture was diluted with 1M aqueous Na2CO3 solution and the phases separated. The aqueous phase was extracted twice with DCM and the combined organic phase was dried (Na2SO4) and evaporated to afford (4-dimethylamino-piperidin-1-yl)-(4-iodo-phenyl)-methanone as a white solid (6.2 g, 98%). LCMS (Method 3) [M+H]+=359.2, RT=1.82 min.

후처리

  1. customthe phases separated
  2. extractionThe aqueous phase was extracted twice with DCM
  3. dry with materialthe combined organic phase was dried (Na2SO4)
  4. customevaporated

출처 및 근거

ORD 기록
ord-84f75af1e6c94959a334d320bd58640e
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09346815B2

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