Benzyl 2-[3-(4-cyanophenoxy)-3-methyl-1-butyn-1-yl]pyridine-5-carboxylate → benzyl 6-(6-cyano-2,2-dimethyl-2H-1-benzopyran-4-yl)-3-pyridinecarboxylate

HRID 1073919

反応式

HRID 1073919 の反応式
[C:1]([C:3]1[CH:30]=[CH:29][C:6]([O:7][C:8]([CH3:28])([CH3:27])[C:9]#[C:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]([O:19][CH2:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)=[O:18])=[CH:13][N:12]=2)=[CH:5][CH:4]=1)#[N:2]>ClC1C=CC=CC=1Cl>[C:1]([C:3]1[CH:30]=[CH:29][C:6]2[O:7][C:8]([CH3:28])([CH3:27])[CH:9]=[C:10]([C:11]3[N:12]=[CH:13][C:14]([C:17]([O:19][CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)=[O:18])=[CH:15][CH:16]=3)[C:5]=2[CH:4]=1)#[N:2]

参加物

3

反応物 1

HCID 19895702Benzyl 2-[3-(4-cyanophenoxy)-3-methyl-1-butyn-1-yl]pyridine-5-carboxylate

生成物 1

HCID 54263699benzyl 6-(6-cyano-2,2-dimethyl-2H-1-benzopyran-4-yl)-3-pyridinecarboxylate収率 61.1%

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒2 回

実験手順

9 g of benzyl 2-[3-(4-cyanophenoxy)-3-methyl-1-butyn-1-yl]pyridine-5-carboxylate were dissolved in 300 ml of 1,2-dichlorobenzene and the solution was added dropwise over a period of 5 hours to 100 ml of 1,2-dichlorobenzene heated at reflux. After a further 2 hours the mixture was allowed to cool to room temperature and was then evaporated. The residue was chromatographed on silica gel using ethyl acetate/petroleum ether (1:9), (1:6) and (1:4) for the elution. There were obtained 5.5 g of benzyl 6-(6 -cyano-2,2-dimethyl-2H-1-benzopyran-4-yl)-3-pyridinecarboxylate which was used without further purification.

後処理

  1. temperatureheated
  2. temperatureat reflux
  3. customwas then evaporated
  4. customThe residue was chromatographed on silica gel
  5. washfor the elution

出典と根拠

ORDレコード
ord-c260eed9a854468887d028f57130df08
出典データセット
uspto-grants-1990_11
特許番号
US04971982

関連ノート

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