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Methyl iodide → 2-Methylthio-3,5-dicyano-4-methoxythiophene

HRID 982015
ノート
印刷プレビュー

反応式

HRID 982015 の反応式
[CH3:1][S:2][C:3]1[S:4][C:5]([C:11]#[N:12])=[C:6]([OH:10])[C:7]=1[C:8]#[N:9].CI.[C:15](=O)([O-])[O-].[K+].[K+].C(N(CC)CC)C>C(#N)C>[CH3:1][S:2][C:3]1[S:4][C:5]([C:11]#[N:12])=[C:6]([O:10][CH3:15])[C:7]=1[C:8]#[N:9]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 141197702-Methylthio-3,5-dicyano-4-hydroxythiophene

生成物 1

HCID 141197712-Methylthio-3,5-dicyano-4-methoxythiophene

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

このページの内容参加物実験手順後処理出典と根拠反応ノート

6 g of 2-methylthio-3,5-dicyano-4-hydroxythiophene 10 ml of methyl iodide, 10 g of potassium carbonate, and 3 ml of triethylamine are refluxed in 300 ml of acetonitrile while stirring. After 2 hours the reaction mixture is filtered warm and evaporated to dryness. The residue is taken up in 200 ml of methylene chloride and washed successively with a solution of potassium carbonate in water and with water. The methylene chloride solution is then dried and evaporated to dryness. After recrystallisation of the residue from isopropanol, the desired product is obtained in a yield of 4.0 g; melting-point 132° C.

後処理

  1. filtrationAfter 2 hours the reaction mixture is filtered
  2. temperaturewarm
  3. customevaporated to dryness
  4. washwashed successively with a solution of potassium carbonate in water and with water
  5. dry with materialThe methylene chloride solution is then dried
  6. customevaporated to dryness
  7. customAfter recrystallisation of the residue from isopropanol

出典と根拠

ORDレコード
ord-0887362eb0574398a66fd717bf5a366f
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04994485

反応ノート

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