Sulfuric Acid → (2,2,2-trifluoroethoxy)acetic acid

HRID 258320노트

반응식

HRID 258320 반응식
[F:1][C:2]([F:11])([F:10])[CH2:3][O:4][CH2:5][C:6]([O:8]C)=[O:7].[OH-].[Na+].S(=O)(=O)(O)O>CO.CCOCC>[F:1][C:2]([F:11])([F:10])[CH2:3][O:4][CH2:5][C:6]([OH:8])=[O:7]

참가 물질

6

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온도
0 °C

실험 절차

To a solution of methyl 2-(2,2,2-trifluoroethoxy)acetate (8.26 g, 47.98 mmol) and methanol (16 mL) was added sodium hydroxide (1.92 g, 47.98 mmol) in methanol (16 mL). After stirring for 18 hours, the reaction was concentrated and ether (170 mL) was added. The mixture was cooled to 0° C. and concentrated sulfuric acid (2.15 g, 43.9 mmol) in ether (7.5 mL) was slowly added. The resulting mixture was stirred for 18 hours, filtered and concentrated to give the title compound as a colorless oil (7.15 g, 94%), MS(CI): 159(M+H); H-NMR (300 MHz, DMSO-d6): 4.14(q, J=9.3 Hz, 2H), 4.21(s, 2H), 12.92(s, 1H).

후처리

  1. concentrationthe reaction was concentrated
  2. additionether (170 mL) was added
  3. stirringThe resulting mixture was stirred for 18 hours
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-302d094745d640789173e56fca20b9cb
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05266570

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