Diisopropylamine → 2-[2-(2-Methoxyethoxymethoxy)ethyl]thiophene

HRID 270656

반응식

HRID 270656 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][CH2:7][OH:8].C(NC(C)C)(C)C.[CH3:16][O:17][CH2:18][CH2:19][O:20][CH2:21]Cl>ClCCl>[CH3:16][O:17][CH2:18][CH2:19][O:20][CH2:21][O:8][CH2:7][CH2:6][C:2]1[S:1][CH:5]=[CH:4][CH:3]=1

참가 물질

5

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온도
0 °C

실험 절차

15.0 g of 2-thiopheneethanol was dissolved in 350 mL of dichloromethane, and 30.2 g of diisopropylamine was added thereto. The resulting mixture was cooled to 0° C. and 17.5 g of 2-methoxyethoxymethyl chloride was added thereto. The resulting mixture was stirred for 2 hours and heated to reflux for 2 hours. The reaction product solution was cooled and concentrated by evaporation under reduced pressure. To the residue, 200 mL of water and 250 mL of n-hexane were added, and the resulting mixture was stirred for 5 minutes. Aqueous layer was discarded, and the organic layer was washed twice with 700 mL portions of water, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 21.5 g (yield of 85%) of the title compound as a colorless oil.

후처리

  1. temperatureheated
  2. temperatureto reflux for 2 hours
  3. temperatureThe reaction product solution was cooled
  4. concentrationconcentrated by evaporation under reduced pressure
  5. additionTo the residue, 200 mL of water and 250 mL of n-hexane were added
  6. stirringthe resulting mixture was stirred for 5 minutes
  7. washthe organic layer was washed twice with 700 mL portions of water
  8. dry with materialdried over anhydrous magnesium sulfate
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e81fb2b8b6d84ee4beb9aff279930772
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449580B2

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