4-(3,4-Dichlorophenoxy)piperidine → tert-Butyl 2-{[4-(3,4-dichlorophenoxy)piperidin-1-yl}methyl]morpholine-4-carboxylate

HRID 2110804노트

반응식

HRID 2110804 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[O:5][CH:6]1[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1.CS(O[CH2:21][C:22]1(CO)[O:27][CH2:26][CH2:25][N:24]([C:28]([O:30][C:31]([CH3:34])([CH3:33])[CH3:32])=[O:29])[CH2:23]1)(=O)=O>C(#N)C>[NH3:9].[Cl:1][C:2]1[CH:3]=[C:4]([CH:12]=[CH:13][C:14]=1[Cl:15])[O:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:21][CH:22]2[O:27][CH2:26][CH2:25][N:24]([C:28]([O:30][C:31]([CH3:32])([CH3:34])[CH3:33])=[O:29])[CH2:23]2)[CH2:8][CH2:7]1

참가 물질

5

반응물 2

HCID 37320424-(3,4-Dichlorophenoxy)piperidineHCID 866286481,1-Dimethylethyl 2-[[(methylsulfonyl)oxy]methyl]-2-(hydroxymethyl)-4-morpholinecarboxylate

생성물 2

HCID 222AmmoniaHCID 17974804tert-Butyl 2-{[4-(3,4-dichlorophenoxy)piperidin-1-yl}methyl]morpholine-4-carboxylate수율 76.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a solution of 4-(3,4-dichlorophenoxy)piperidine (WO 01/77101; 9.22 g) dissolved in acetonitrile (60 ml) was added the product of Step (a) (5.53 g). The mixture was refluxed for 12 hrs and the solvents were evaporated. Purification by flash chromatography eluting with dichloromethane:methanol:NH3 (aq) (2:97.9:0.1) gave the sub-title compound as an oil (5.76 g).

후처리

  1. temperatureThe mixture was refluxed for 12 hrs
  2. customthe solvents were evaporated
  3. customPurification by flash chromatography
  4. washeluting with dichloromethane

출처 및 근거

ORD 기록
ord-a5057c5d45694d73a49d77ba26bb1865
출처 데이터셋
uspto-grants-2009_04
특허 번호
US07517989B2

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