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Sodium Iodide → 4-(1-Ethoxyethoxy)-3,3-difluoro-1-iodo-4-methylpentane

HRID 745640
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HRID 745640 반응식
CC1C=CC(S(O[CH2:12][CH2:13][C:14]([F:25])([F:24])[C:15]([O:18][CH:19]([O:21][CH2:22][CH3:23])[CH3:20])([CH3:17])[CH3:16])(=O)=O)=CC=1.C(N(C(C)C)CC)(C)C.[I-:35].[Na+]>CC(C)=O>[CH2:22]([O:21][CH:19]([O:18][C:15]([CH3:17])([CH3:16])[C:14]([F:25])([F:24])[CH2:13][CH2:12][I:35])[CH3:20])[CH3:23]
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참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 81531DiisopropylethylamineHCID 13189250HCID 13189250, 화합물

생성물 1

HCID 131892514-(1-Ethoxyethoxy)-3,3-difluoro-1-iodo-4-methylpentane

시약·촉매·용매 1

HCID 180Acetone용매

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온도
25 °C

실험 절차

A mixture of 3.50 g (0.0087 mol) of 4-(1-ethoxyethoxy)-3,3-difluoro-4-methyl-1-pentanol 1-(4-methylbenzenesulfonate), 40 mL of acetone, 0.5 mL of diisopropylethylamine and 13.10 g (0.087 mol) of sodium iodide was stirred at 25° C. for 64 hr. The mixture was evaporated to dryness. The residue was partitioned between 5% aqueous sodium sulfite solution and methylene chloride. The organic phase was washed with saturated aqueous sodium bicarbonate solution. The organic phase was then dried over anhydrous magnesium sulfate, filtered, and evaporated to dryness. The residue was chromatographed on 0.06-0.20 mm silica gel to yield 4-(1-ethoxyethoxy)-3,3-difluoro-1-iodo-4-methylpentane.

후처리

  1. customThe mixture was evaporated to dryness
  2. customThe residue was partitioned between 5% aqueous sodium sulfite solution and methylene chloride
  3. washThe organic phase was washed with saturated aqueous sodium bicarbonate solution
  4. dry with materialThe organic phase was then dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customevaporated to dryness
  7. customThe residue was chromatographed on 0.06-0.20 mm silica gel

출처 및 근거

ORD 기록
ord-3fc57feef96545efa058f46a13aa7d69
출처 데이터셋
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04599330

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