Sodium Iodide → HCID 53645944, 화합물

HRID 725596노트

반응식

HRID 725596 반응식
[OH:1][C:2]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH2:15](Br)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[I-].[Na+]>CC(C)=O>[CH2:15]([O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])=[CH:10][C:2]=1[O:1][CH2:4][C:3]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:2]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 7498Benzyl BromideHCID 10796Cesium carbonateHCID 4330244-tert-Butyl-2-hydroxybenzoic acid

생성물 1

HCID 53645944HCID 53645944, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 5 g of 2-hydroxy-4-tert-butyl-benzoic acid, 9.1 ml of benzyl bromide, 17 g of caesium carbonate, 0.3 g of sodium iodide and 500 ml of acetone is stirred for 20 hours under reflux and then filtered and the filtrate is concentrated by evaporation. The residue is partitioned between diethyl ether and water, the organic phases are concentrated by evaporation and the residue is purified by means of FC (1000 g of silica gel, dichloromethane/hexane=1:1). Title compound: Rf (dichloromethane/hexane=1:1)=0.47.

후처리

  1. temperatureunder reflux
  2. filtrationfiltered
  3. concentrationthe filtrate is concentrated by evaporation
  4. customThe residue is partitioned between diethyl ether and water
  5. concentrationthe organic phases are concentrated by evaporation
  6. customthe residue is purified by means of FC (1000 g of silica gel, dichloromethane/hexane=1:1)

출처 및 근거

ORD 기록
ord-94c42cb43941478b81faf87bb6aedd1e
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05705658

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