Piperidine → HCID 59835795、化合物

HRID 1916695ノート

反応式

HRID 1916695 の反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.CS(O[CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([C:21]#[C:22][C:23]2[CH:28]=[CH:27][C:26]([C:29]3[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][CH:30]=3)=[CH:25][N:24]=2)=[CH:17][CH:16]=1)(=O)=O>CN(C=O)C>[Cl:35][C:32]1[CH:33]=[CH:34][C:29]([C:26]2[CH:27]=[CH:28][C:23]([C:22]#[C:21][C:18]3[CH:19]=[CH:20][C:15]([O:14][CH2:13][CH2:12][N:1]4[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]4)=[CH:16][CH:17]=3)=[N:24][CH:25]=2)=[CH:30][CH:31]=1

参加物

4

反応物 2

HCID 8082PiperidineHCID 86601132HCID 86601132、化合物

生成物 1

HCID 59835795HCID 59835795、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

99 μL (1.0 mmol) piperidine are added to a solution of 85.6 mg (0.2 mmol) of 2-{4-[5-(4-chloro-phenyl)-pyridin-2-ylethynyl]-phenoxy}-ethyl methanesulphonate in 2 mL DMF and the reaction mixture is stirred for 18 h at RT. The solvent is distilled off i.vac., the residue is stirred with 5 mL water and 40 mL DCM, the organic phase is separated off and dried with Na2SO4. After the desiccant and solvent have been eliminated the residue is triturated with 20 mL diethyl ether and suction filtered.

後処理

  1. distillationThe solvent is distilled off i.vac
  2. stirring, the residue is stirred with 5 mL water and 40 mL DCM
  3. customthe organic phase is separated off
  4. dry with materialdried with Na2SO4
  5. customis triturated with 20 mL diethyl ether and suction
  6. filtrationfiltered

出典と根拠

ORDレコード
ord-a16706884bd94511a5aff1ec8201bdbd
出典データセット
uspto-grants-2013_12
特許番号
US08618132B2

反応ノート

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