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Methyl iodide → HCID 1704453, 화합물

HRID 1049155
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HRID 1049155 반응식
[C:1](#[N:5])[CH2:2][C:3]#[N:4].[C:6]1([N:12]=[C:13]=[S:14])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[CH3:15]I>CN(C=O)C>[CH3:15][S:14][C:13]([NH:12][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[C:2]([C:1]#[N:5])[C:3]#[N:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 7673Phenyl IsothiocyanateHCID 8010Malononitrile

생성물 1

HCID 1704453HCID 1704453, 화합물수율 99%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of malononitrile (1.0 g, 15.14 mmol) in DMF 20 mL was added TEA (2.099 mL, 15.14 mmol). After the mixture was stirred at room temperature for 5 min, phenylisothiocynate (2.047 g, 15.14 mmol) was added dropwise to the mixture. The reaction mixture was stirred at room temperature for 30 min. After the reaction was complete as determined by TLC, methyl iodide (2.149 g, 15.14 mmol) was added and the reaction mixture was stirred at room temperature for 1 hr, at which time the reaction was complete as determined by TLC. The reaction mixture was poured into 100 mL ice water. The resulting precipitate was filtered and dried in an oven overnight to give compound 6 (3.226 g, 98.2% yield, 97.4% purity) as a light yellow solid.

후처리

  1. stirringThe reaction mixture was stirred at room temperature for 30 min
  2. additionwas added
  3. stirringthe reaction mixture was stirred at room temperature for 1 hr, at which time the reaction
  4. filtrationThe resulting precipitate was filtered
  5. customdried in an oven overnight

출처 및 근거

ORD 기록
ord-6fed7941a26a4d6fba946040bdb6e8ad
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382237B2

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