Dimethoxymethane → 2-Bromo-4-fluoro-1-(methoxymethoxy)benzene

HRID 2069897노트

반응식

HRID 2069897 반응식
[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[OH:9].[CH3:10][O:11][CH2:12]OC.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.[OH-].[Na+]>ClCCl>[Br:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[O:9][CH2:10][O:11][CH3:12]

참가 물질

6

반응물 4

HCID 8020DimethoxymethaneHCID 14798Sodium HydroxideHCID 14812Phosphorus oxide (P4O10)HCID 6054722-Bromo-4-fluorophenol

생성물 1

HCID 220325852-Bromo-4-fluoro-1-(methoxymethoxy)benzene수율 98.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Bromo-4-fluorophenol (25.0 g, 0.13 mol) was dissolved in dry dichloromethane (100 mL) and dimethoxymethane (115 mL, 1.30 mol). Phosphorus pentoxide (110.8 g, 0.39 mol) was added portion-wise to the solution such that the reaction temperature remained below 40° C. The mixture was stirred vigorously at room temperature for 2 hours and then carefully poured into 1N aqueous NaOH (50 mL). The organic layer was separated, washed with water and then brine, dried over anhydrous MgSO4, filtered and concentrated to give 2-bromo-4-fluoro-1-methoxymethoxy-benzene (30.1 g) as a colorless oil.

후처리

  1. customremained below 40° C
  2. customThe organic layer was separated
  3. washwashed with water
  4. dry with materialbrine, dried over anhydrous MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-cc77edee348a474ca5c1249fa0e29a5d
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08299110B2

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