Iodine → HCID 18979647, 화합물

HRID 1080562노트

반응식

HRID 1080562 반응식
C([Li])CCC.[CH2:6]([C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[C:11]([F:16])[CH:10]=1)[CH2:7][CH3:8].[I:17]I.C(=O)(O)[O-].[Na+]>CCCCCC.O1CCCC1>[CH2:6]([C:9]1[CH:10]=[C:11]([F:16])[C:12]([I:17])=[C:13]([F:15])[CH:14]=1)[CH2:7][CH3:8]

참가 물질

7

반응물 4

HCID 807IodineHCID 516892Sodium BicarbonateHCID 189796611,3-Difluoro-5-propylbenzeneHCID 178418339Butyllithium

생성물 1

HCID 18979647HCID 18979647, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매

실험 절차

22 ml of a 1.6N butyllithium solution in hexane were added dropwise during 30 min. to a solution of 5 g of 1-propyl-3,5-difluorobenzene in 50 ml of dry tetrahydrofuran at -70° C. and left to react at -70° C. for 1 hour. Then, a solution of 8.95 g of iodine in 20 ml of dry tetrahydrofuran was added dropwise at -60° within 10 minutes and the mixture was gradually warmed to room temperature within a further 30 minutes. The resulting yellow solution was then treated with 40 ml of a 10 percent aqueous sodium bicarbonate solution and extracted with ether. The ether solution was washed with saturated sodium chloride solution and several times with water, dried over magnesium sulphate, filtered and concentrated. Chromatography of the residue over 200 g of silica gel with hexane gave 1-propyl-3,5-difluoro-4-iodobenzene as a colourless liquid.

후처리

  1. waitleft
  2. customto react at -70° C. for 1 hour
  3. extractionextracted with ether
  4. washThe ether solution was washed with saturated sodium chloride solution and several times with water
  5. dry with materialdried over magnesium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-c49e50a67cdc4273a899439b5ad1e423
출처 데이터셋
uspto-grants-1996_12
특허 번호
US05582767

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