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

HRID 1073966노트

반응식

HRID 1073966 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4b11f7d6bccc4a2cb1e8bbaa02bb8e4d
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971982

반응 노트

불러오는 중…