Water → HCID 13367596, 화합물

HRID 1583587노트

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HRID 1583587 반응식
[F:1][CH2:2][CH2:3][O:4][C:5]1[CH:6]=[C:7]([CH:10]=[CH:11][CH:12]=1)[CH2:8]Cl.[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([C:20]([CH3:24])([CH3:23])[CH2:21][OH:22])=[CH:16][CH:15]=1.[OH-].[Na+].O>[Br-].C([N+](CC)(CC)CC1C=CC=CC=1)C.C1(C)C=CC=CC=1>[Cl:13][C:14]1[CH:15]=[CH:16][C:17]([C:20]([CH3:24])([CH3:23])[CH2:21][O:22][CH2:8][C:7]2[CH:10]=[CH:11][CH:12]=[C:5]([O:4][CH2:3][CH2:2][F:1])[CH:6]=2)=[CH:18][CH:19]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 130345572-(4-Chlorophenyl)-2-methylpropanolHCID 135356311-(Chloromethyl)-3-(2-fluoroethoxy)benzene

생성물 1

HCID 13367596HCID 13367596, 화합물수율 81.2%

시약·촉매·용매 2

HCID 165294Benzyltriethylammonium bromide촉매HCID 1140Toluene용매

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온도
50 °C

실험 절차

A mixture consisting of 2.0 g of 3-(2-fluoroethoxy)benzyl chloride, 2.3 g of 2-(4-chlorophenyl)-2-methylpropyl alcohol, 0.5 g of triethylbenzylammonium bromide and 5 g of a 50% aqueous solution of sodium hydroxide was stirred at 50° C. for 2 hours. The reaction mixture was cooled to room temperature, and poured into water. Toluene was added, and the mixture was fully stirred. The toluene layer was separated, washed with water and dried over anhydrous sodium sulfate. Toluene was evaporated under reduced pressure. The resulting crude ether was purified by silica gel (100 g) column chromatography (developing solvent: toluene) to give 2.9 g of the desired 3-(2-fluoroethoxy)benzyl 2-(4-chlorophenyl)-2-methylpropyl ether.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. stirringthe mixture was fully stirred
  3. customThe toluene layer was separated
  4. washwashed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customToluene was evaporated under reduced pressure
  7. customThe resulting crude ether was purified by silica gel (100 g) column chromatography (developing solvent: toluene)

출처 및 근거

ORD 기록
ord-e1c85974654444868703021f7b53b3c6
출처 데이터셋
uspto-grants-1985_11
특허 번호
US04552894

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