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

HRID 2110804ノート

反応式

HRID 2110804 の反応式
[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

参加物

5

反応物 2

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

生成物 2

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-a5057c5d45694d73a49d77ba26bb1865
出典データセット
uspto-grants-2009_04
特許番号
US07517989B2

反応ノート

読み込み中…