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

반응식

HRID 892556 반응식
[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]

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-30fd7b3a6cf04131a840548e7ff02b2c
출처 데이터셋
uspto-grants-1992_06
특허 번호
US05118694

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