Hydrochloric Acid → HCID 15058702、化合物

HRID 1087899

反応式

HRID 1087899 の反応式
[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]

参加物

7

反応物 5

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

生成物 1

HCID 15058702HCID 15058702、化合物収率 51%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94f77d4fec884cf2aa5ba069745f4405
出典データセット
uspto-grants-1990_10
特許番号
US04960884

関連ノート

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