Potassium Iodide → HCID 68829534、化合物

HRID 747776ノート

反応式

HRID 747776 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([NH2:21])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Br[CH2:23][CH2:24][O:25][C:26]1[CH:27]=[C:28]([CH:31]=[CH:32][CH:33]=1)[C:29]#[N:30].[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([NH:21][CH2:23][CH2:24][O:25][C:26]3[CH:27]=[C:28]([CH:31]=[CH:32][CH:33]=3)[C:29]#[N:30])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 177889413-(2-bromoethoxy)benzonitrileHCID 22181157tert-Butyl 4-(4-aminophenoxy)piperidine-1-carboxylate

生成物 1

HCID 68829534HCID 68829534、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

616 mg (1.91 mmol) of 1-t-butoxycarbonyl-4-(4-aminophenoxy)piperidine, 432 ml (1.91 mmol) of 3-(2-bromoethoxy)benzonitrile and 634 mg (3.82 mmol) of potassium iodide were dissolved in 20 ml of dimethylformamide. 2.64 g (19.1 mmol) of potassium carbonate was added to the solution, and they were stirred at room temperature for 14 hours. The solvent was distilled off under reduced pressure. After the treatment with ethyl acetate as extractant in an ordinary manner, the crude product was obtained. This product was purified by the silica gel column chromatography to obtain the title compound.

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. customAfter the treatment with ethyl acetate as extractant in an ordinary manner, the crude product was obtained
  3. customThis product was purified by the silica gel column chromatography

出典と根拠

ORDレコード
ord-21442828d21b4c33bd0871afa108cb0f
出典データセット
uspto-grants-2008_07
特許番号
US07396844B1

反応ノート

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