Potassium Carbonate → HCID 86659378、化合物

HRID 1187676

反応式

HRID 1187676 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([Cl:10])[N:9]=1)[CH:5]=[O:6].C1(C)C=CC(S([CH2:20][N+:21]#[C-:22])(=O)=O)=CC=1.C(=O)([O-])[O-].[K+].[K+]>CO>[Cl:1][C:2]1[CH:3]=[C:4]([C:5]2[O:6][CH:22]=[N:21][CH:20]=2)[CH:7]=[C:8]([Cl:10])[N:9]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 161915Tosylmethyl isocyanideHCID 27610242,6-Dichloropyridine-4-carbaldehyde

生成物 1

HCID 86659378HCID 86659378、化合物収率 97.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
50 °C

実験手順

528 mg of 2,6-dichloroisonicotinaldehyde (this compound was prepared by the method described in J. Chem. Soc., Chem. Commun., 1998, 1567-1568) was dissolved in 10 ml of methanol, and 586 mg of p-toluenesulfonyl methyl isocyanide and 415 mg of potassium carbonate ware added, and the mixture was stirred at 50° C. for 30 minutes. The reaction solution was concentrated, and then diluted with ethyl acetate, and the organic layer was washed with a saturated aqueous solution of sodium bicarbonate and brine, and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 630 mg of the objective compound as white powder.

後処理

  1. concentrationThe reaction solution was concentrated
  2. additiondiluted with ethyl acetate
  3. washthe organic layer was washed with a saturated aqueous solution of sodium bicarbonate and brine
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-e49229dca49d4e5b89648b03d2c88c00
出典データセット
uspto-grants-2014_03
特許番号
US08673891B2

関連ノート

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