Iodine → HCID 66733550, 화합물

HRID 403011

반응식

HRID 403011 반응식
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([CH:14]=[CH:15][C:16]=1[O:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:12][OH:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[I:25]I>C(Cl)(Cl)Cl.FC(F)(F)C([O-])=O.[Ag+]>[CH2:1]([O:8][C:9]1[CH:10]=[C:11]([C:14]([I:25])=[CH:15][C:16]=1[O:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:12][OH:13])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 2

HCID 807IodineHCID 743383,4-Bis(benzyloxy)benzyl alcohol

생성물 1

HCID 66733550HCID 66733550, 화합물수율 84%

시약·촉매·용매 2

HCID 76299Silver trifluoroacetate촉매HCID 6212Chloroform용매2회

실험 절차

The dibenzyloxybenzyl alcohol 28 (21.44 mmol) and silver trifluoroacetate (21.44 mmol) were suspended in 100 mL of dry chloroform and stirred under argon. A solution of iodine (21.44 mmol) in dry chloroform (50 mL) was added to the suspension dropwise at room temperature. The reaction mixture was then stirred for a further period of 2 h and filtered. The filtrate was washed with 20% sodium thiosulfate solution in water. The organic layer was separated and dried over anhydrous Na2SO4. Filtration was followed by evaporation of the chloroform solution resulting in the pure iodo compound, 3,4-Dibenzyloxy-6-iodobenzyl alcohol (29), as a pale yellow solid in 84% yield.

후처리

  1. stirringThe reaction mixture was then stirred for a further period of 2 h
  2. filtrationfiltered
  3. washThe filtrate was washed with 20% sodium thiosulfate solution in water
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationFiltration
  7. customwas followed by evaporation of the chloroform solution

출처 및 근거

ORD 기록
ord-ecb27ec953764accb3730e698a8568d6
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08742139B2

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