[3-Cyano-4,5-dimethyl-5-(trifluoromethyl)furan-2(5H)-ylidene]malononitrile → 2-[4-[2-[4-[2-(4-dibutylamino-2-methoxyphenyl)vinyl]phenyl]vinyl]-3-cyano-5-methyl-5-trifluoromethyl-2(5H)-furanylidene]propanedinitrile

HRID 85252ノート

反応式

HRID 85252 の反応式
[CH2:1]([N:5]([CH2:24][CH2:25][CH2:26][CH3:27])[C:6]1[CH:11]=[CH:10][C:9]([CH:12]=[CH:13][C:14]2[CH:21]=[CH:20][C:17]([CH:18]=O)=[CH:16][CH:15]=2)=[C:8]([O:22][CH3:23])[CH:7]=1)[CH2:2][CH2:3][CH3:4].[C:28]([C:30]1[C:31](=[C:41]([C:44]#[N:45])[C:42]#[N:43])[O:32][C:33]([CH3:40])([C:36]([F:39])([F:38])[F:37])[C:34]=1[CH3:35])#[N:29]>C(O)C.O1CCCC1>[CH2:24]([N:5]([CH2:1][CH2:2][CH2:3][CH3:4])[C:6]1[CH:11]=[CH:10][C:9]([CH:12]=[CH:13][C:14]2[CH:21]=[CH:20][C:17]([CH:18]=[CH:35][C:34]3[C:33]([CH3:40])([C:36]([F:39])([F:37])[F:38])[O:32][C:31](=[C:41]([C:42]#[N:43])[C:44]#[N:45])[C:30]=3[C:28]#[N:29])=[CH:16][CH:15]=2)=[C:8]([O:22][CH3:23])[CH:7]=1)[CH2:25][CH2:26][CH3:27]

参加物

5

反応物 2

HCID 22020292[3-Cyano-4,5-dimethyl-5-(trifluoromethyl)furan-2(5H)-ylidene]malononitrileHCID 866675494-[2-(4-Dibutylamino-2-methoxyphenyl)vinyl]benzaldehyde

生成物 1

HCID 866675512-[4-[2-[4-[2-(4-dibutylamino-2-methoxyphenyl)vinyl]phenyl]vinyl]-3-cyano-5-methyl-5-trifluoromethyl-2(5H)-furanylidene]propanedinitrile収率 38.9%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

In 15 ml of ethanol and 5 ml of tetrahydrofuran were dissolved 500 mg (1.37 mmol) of 4-[2-(4-dibutylamino-2-methoxyphenyl)vinyl]benzaldehyde and 380 mg (1.50 mmol) of 2-(3-cyano-4,5-dimethyl-5-trifluoromethyl-2(5H)-furanylidene)propanedinitrile. The mixture was stirred at 50° C. for 9 hours. The solvent was evaporated off and the residue was washed with ethanol. The residue was purified by silica gel column chromatography and washed with ethanol to give 320 mg of a black powder (yield: 38.9%; mp: 175-177° C.)

後処理

  1. customThe solvent was evaporated off
  2. washthe residue was washed with ethanol
  3. customThe residue was purified by silica gel column chromatography
  4. washwashed with ethanol

出典と根拠

ORDレコード
ord-4610b66c2b444bdd9274c7b03856e42d
出典データセット
uspto-grants-2014_09
特許番号
US08846955B2

反応ノート

読み込み中…