Methyl iodide → HCID 54010899, 화합물

HRID 2165217노트

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HRID 2165217 반응식
[CH3:1]I.[Mg].C[C:5]1[C:12]([F:13])=[C:11]([F:14])[C:8]([CH:9]=[O:10])=[C:7]([F:15])[C:6]=1[F:16].[Cl-].[NH4+]>C(OCC)C>[CH3:1][CH:9]([OH:10])[C:8]1[C:7]([F:15])=[C:6]([F:16])[CH:5]=[C:12]([F:13])[C:11]=1[F:14]

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 132680124-Methyl-2,3,5,6-tetrafluoro-benzaldehyde

생성물 1

HCID 54010899HCID 54010899, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

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온도
0 °C

실험 절차

3 2 ml of methyl iodide were introduced over the course of 30 minutes into a suspension of 1 g of magnesium and 30 ml of ethyl ether and the mixture was stirred for 30 minutes. The mixture was cooled to 0° C. and 4 g of 4-methyl-2,3,5,6-tetra fluorobenzaldehyde and 100 ml of ethyl ether were introduced over the course of 30 minutes. The reaction mixture was stirred for 1 hour at 0° C. and was poured into 150 ml of a saturated aqueous ammonium chloride solution. Extraction was carried out with ether and the ethereal phases were dried and evaporated to dryness under reduced pressure. The crude product was chromatographed on silica and eluted with a hexane:isopropyl ether (8:2) mixture to obtain 3.85 g of the product with a Rf=0.10.

후처리

  1. stirringThe reaction mixture was stirred for 1 hour at 0° C.
  2. extractionExtraction
  3. customthe ethereal phases were dried
  4. customevaporated to dryness under reduced pressure
  5. customThe crude product was chromatographed on silica
  6. washeluted with a hexane:isopropyl ether (8:2) mixture

출처 및 근거

ORD 기록
ord-4b24874aac494aa9a688b1d0ad96eb3c
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04939172

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