4-[1,1-Dimethyl-3-(2-methoxyphenyl)-2-propynyloxy]benzonitrile → 4-(2-methoxyphenyl)-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile

HRID 1073966ノート

反応式

HRID 1073966 の反応式
[CH3:1][C:2]([CH3:22])([O:13][C:14]1[CH:21]=[CH:20][C:17]([C:18]#[N:19])=[CH:16][CH:15]=1)[C:3]#[C:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[O:11][CH3:12]>ClC1C=CC=CC=1Cl>[CH3:12][O:11][C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=1[C:4]1[C:21]2[CH:20]=[C:17]([C:18]#[N:19])[CH:16]=[CH:15][C:14]=2[O:13][C:2]([CH3:22])([CH3:1])[CH:3]=1

参加物

3

反応物 1

HCID 198956454-[1,1-Dimethyl-3-(2-methoxyphenyl)-2-propynyloxy]benzonitrile

生成物 1

HCID 198955864-(2-methoxyphenyl)-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile収率 48.5%

試薬・触媒・溶媒 1

HCID 72391,2-Dichlorobenzene溶媒

実験手順

0.99 g of 4-[1,1-dimethyl-3-(2-methoxyphenyl)-2-propynyloxy]benzonitrile was dissolved in 10 ml of 1,2-dichlorobenzene and heated at reflux for 1.5 hours. After cooling the solution was evaporated and the residue was chromatographed on silica gel using ethyl acetate/petroleum ether (1:4) for the elution. After recrystallization from petroleum ether (boiling point 60°-80° C.) there were obtained 480 mg of 4-(2-methoxyphenyl)-2,2-dimethyl-2H-1-benzopyran-6-carbonitrile of melting point 109°-111° C.

後処理

  1. temperatureheated
  2. temperatureat reflux for 1.5 hours
  3. temperatureAfter cooling the solution
  4. customwas evaporated
  5. customthe residue was chromatographed on silica gel
  6. washfor the elution
  7. customAfter recrystallization from petroleum ether (boiling point 60°-80° C.) there

出典と根拠

ORDレコード
ord-4b11f7d6bccc4a2cb1e8bbaa02bb8e4d
出典データセット
uspto-grants-1990_11
特許番号
US04971982

反応ノート

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