Iodine → HCID 18979647、化合物

HRID 1080562ノート

反応式

HRID 1080562 の反応式
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]

参加物

7

反応物 4

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

生成物 1

HCID 18979647HCID 18979647、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8058Hexane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c49e50a67cdc4273a899439b5ad1e423
出典データセット
uspto-grants-1996_12
特許番号
US05582767

反応ノート

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