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 892556

反応式

HRID 892556 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 10% 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-30fd7b3a6cf04131a840548e7ff02b2c
出典データセット
uspto-grants-1992_06
特許番号
US05118694

関連ノート

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