Hydrochloric Acid → HCID 66858654, 화합물

HRID 1803149노트

반응식

HRID 1803149 반응식
Cl[C:2]([O:4][CH2:5][CH3:6])=[O:3].[F:7][C:8]1[C:13]([F:14])=[CH:12][CH:11]=[CH:10][C:9]=1[OH:15].C(N(CC)CC)C.Cl>CCOC(C)=O>[C:2](=[O:3])([O:4][CH2:5][CH3:6])[O:15][C:9]1[CH:10]=[CH:11][CH:12]=[C:13]([F:14])[C:8]=1[F:7]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 808792,3-Difluorophenol

생성물 1

HCID 66858654HCID 66858654, 화합물수율 64.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Step M (1): Ethyl chloroformate (16.6 g, 153 mmol) was added to a solution of 2,3-difluorophenol (20 g, 153 mmol) and triethylamine (20.7 mL, 146 mmol) in EtOAc (200 mL). The resulting mixture was stirred at rt for 2 h. The crude reaction was poured into 1 N HCl and extracted with EtOAc. The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo. The residue was purified using silica gel column chromatography (5% EtOAc/hexane) to afford 2,3-difluorophenyl ethyl carbonate (20 g, 64% yield).

후처리

  1. customThe crude reaction
  2. extractionextracted with EtOAc
  3. washThe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified

출처 및 근거

ORD 기록
ord-862ab532795748cb80fd783f06c702c2
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08349880B2

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