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

HRID 982015
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HRID 982015 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트

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.

후처리

  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

출처 및 근거

ORD 기록
ord-0887362eb0574398a66fd717bf5a366f
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04994485

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