Iodine → 1-Pyrazolyl iodopropargyl ether

HRID 652698노트

반응식

HRID 652698 반응식
[I:1]I.[CH2:3]([O:6][N:7]1[CH:11]=[CH:10][CH:9]=[N:8]1)[C:4]#[CH:5].C(=O)([O-])[O-].[Na+].[Na+]>C(#N)C>[I:1][CH:3]([O:6][N:7]1[CH:11]=[CH:10][CH:9]=[N:8]1)[C:4]#[CH:5]

참가 물질

5

반응물 3

HCID 807IodineHCID 10340Sodium CarbonateHCID 201962031-Pyrazolyl propargyl ether

생성물 1

HCID 201961981-Pyrazolyl iodopropargyl ether수율 99%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

41.6 g of iodine are added, a little at a time, to 20 g of 1-pyrazolyl propargyl ether and 20 g of sodium carbonate in 400 g of acetonitrile at 40° C., while stirring. Stirring is continued for 8 hours at 40° C., after which undissolved material is filtered off under suction, and the filtrate is evaporated down in a rotary evaporator at 30° C. and under 20 mbar. The residue is dissolved in 200 g of dichloromethane, the solution is extracted twice with 200 g of 10% strength aqueous sodium thiosulfate solution, and the organic phase is dried with magnesium sulfate and evaporated down. 40 g (99% of theory) of 1-pyrazolyl iodopropargyl ether are obtained as an oil (H1 --NMR, in ppm: 5.1, s, 2H; 6.2, m, 1H; 7.4, m, 2H).

후처리

  1. filtrationafter which undissolved material is filtered off under suction
  2. customthe filtrate is evaporated down in a rotary evaporator at 30° C. and under 20 mbar
  3. dissolutionThe residue is dissolved in 200 g of dichloromethane
  4. extractionthe solution is extracted twice with 200 g of 10% strength aqueous sodium thiosulfate solution
  5. dry with materialthe organic phase is dried with magnesium sulfate
  6. customevaporated down

출처 및 근거

ORD 기록
ord-ec7c0d6077134811a13af3487d0043fc
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673429

반응 노트

불러오는 중…