1-Bromo-3-chloropropane → 1-(3-Chloropropoxy)-4-fluoro-2-(phenylmethoxy)benzene

HRID 1761492

반응식

HRID 1761492 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[C:4]([O:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:3]=1.Br[CH2:18][CH2:19][CH2:20][Cl:21].[OH-].[Na+]>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.O>[Cl:21][CH2:20][CH2:19][CH2:18][O:8][C:5]1[CH:6]=[CH:7][C:2]([F:1])=[CH:3][C:4]=1[O:9][CH2:10][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1

참가 물질

6

반응물 3

HCID 80061-Bromo-3-chloropropaneHCID 14798Sodium HydroxideHCID 212415852-(Benzyloxy)-4-fluorophenol

생성물 1

HCID 212416191-(3-Chloropropoxy)-4-fluoro-2-(phenylmethoxy)benzene수율 100%

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 962Water용매

반응 조건

온도
70 °C

실험 절차

To a stirred mixture of 2.5 parts of 4-fluoro-2-(phenylmethoxy)phenol, 2.3 parts of 1-bromo-3-chloropropane, 10 parts of water and 0.39 parts of tetrabutylammonium hydrogen sulfate was added dropwise a solution of 0.7 parts of sodium hydroxide in 5 parts of D at 60° C. (exothermic reaction: temperature rose to 70°). The whole was stirred for 2 hours at 70° C. After cooling, the product was extracted twice with methylbenzene. The combined extracts were dried, filtered and evaporated, yielding 3.4 parts (100%) of 1-(3-chloropropoxy)-4-fluoro-2-(phenylmethoxy)benzene as a residue (intermediate 78).

후처리

  1. custom(exothermic reaction: temperature rose to 70°)
  2. temperatureAfter cooling
  3. extractionthe product was extracted twice with methylbenzene
  4. customThe combined extracts were dried
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-a91fff36e1194381b9a1917a182e6b74
출처 데이터셋
uspto-grants-1989_05
특허 번호
US04826848

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