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Dimethylformamide dimethyl acetal → 4-(3-Dimethylamino-acryloyl)-3-methyl-5-methylsulfanylthiophene-2-carbonitrile

HRID 478181
ノート
印刷プレビュー

反応式

HRID 478181 の反応式
[C:1]([C:4]1[C:5]([CH3:13])=[C:6]([C:11]#[N:12])[S:7][C:8]=1[S:9][CH3:10])(=[O:3])[CH3:2].[CH3:14][N:15]([CH:17](OC)OC)[CH3:16]>C(#N)C>[CH3:14][N:15]([CH3:17])[CH:16]=[CH:2][C:1]([C:4]1[C:5]([CH3:13])=[C:6]([C:11]#[N:12])[S:7][C:8]=1[S:9][CH3:10])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 28201864-Acetyl-3-methyl-5-(methylthio)thiophene-2-carbonitrile

生成物 1

HCID 5360484-(3-Dimethylamino-acryloyl)-3-methyl-5-methylsulfanylthiophene-2-carbonitrile

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a solution of 4-acetyl-3-methyl-5-methylsulfanyl-thiophene-2-carbonitrile (10 mmol) in acetonitrile (5 mL) was added DMF-DMA (2 mL) and the resulting mixture heated at reflux for 18 hours. The reaction was concentrated and the residue triturated with diethyl ether (20 mL). The suspension was filtered and washed with ether to afford the desired product as a yellow solid.

後処理

  1. temperaturethe resulting mixture heated
  2. temperatureat reflux for 18 hours
  3. concentrationThe reaction was concentrated
  4. customthe residue triturated with diethyl ether (20 mL)
  5. filtrationThe suspension was filtered
  6. washwashed with ether

出典と根拠

ORDレコード
ord-950cf2324e5e476fbb96a1f067bfa35a
出典データセット
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06642227B2

反応ノート

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