Hydrochloric Acid → HCID 15058702, 화합물

HRID 1087899

반응식

HRID 1087899 반응식
[OH-].[Na+].[F:3][CH2:4][CH2:5][O:6][C:7]1[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH2:20][CH2:21][F:22])[C:8]=1[C:9]([O:11]CCF)=[O:10].OC1C=CC=C(O)C=1C(O)=O.BrCCF.Cl>C(O)C>[F:3][CH2:4][CH2:5][O:6][C:7]1[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH2:20][CH2:21][F:22])[C:8]=1[C:9]([OH:11])=[O:10]

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 93382,6-Dihydroxybenzoic AcidHCID 129822-Fluoroethyl bromideHCID 14798Sodium HydroxideHCID 15058703HCID 15058703, 화합물

생성물 1

HCID 15058702HCID 15058702, 화합물수율 51%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a stirred solution of 3.0 grams (0.075 mole) of sodium hydroxide in 150 ml of ethanol was added 11.3 grams (0.039 mole) of 2-fluoroethyl 2,6-di(2-fluoroethoxy)benzoate (prepared by the method of Step A of Example 13 from 2,6-dihydroxybenzoic acid and three equivalents of 1-bromo-2-fluoroethane). The reaction mixture was stirred at room temperature for approximately 48 hours. The reaction mixture was filtered, and the filter cake was saved. The filtrate was evaporated under reduced pressure leaving a residue. The filter cake and residue were added to 200 ml of an aqueous, 10% hydrochloric acid solution. The resultant mixture was stirred at room temperature and was extracted with several portions of methylene chloride. The extracts were combined and dried over anhydrous magnesium sulfate. The dried organic phase was filtered, and the filtrate was evaporated under reduced pressure to yield 4.9 grams of 2,6-di(2-fluoroethoxy)benzoic acid as a solid, mp 57°-58° C.

후처리

  1. filtrationThe reaction mixture was filtered
  2. customThe filtrate was evaporated under reduced pressure
  3. customleaving a residue
  4. extractionwas extracted with several portions of methylene chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationThe dried organic phase was filtered
  7. customthe filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-94f77d4fec884cf2aa5ba069745f4405
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960884

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