Ethanone, 1-[3-methoxy-4-(methoxymethoxy)phenyl]- → HCID 59643063, 화합물

HRID 2251611노트

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HRID 2251611 반응식
[Li][CH2:2]CCC.[CH3:6][O:7][C:8]1[CH:9]=[C:10]([C:18](=O)[CH3:19])[CH:11]=[CH:12][C:13]=1[O:14][CH2:15][O:16][CH3:17]>[Br-].C[P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.C1COCC1.CCCCCC>[C:18]([C:10]1[CH:11]=[CH:12][C:13]([O:14][CH2:15][O:16][CH3:17])=[C:8]([O:7][CH3:6])[CH:9]=1)([CH3:19])=[CH2:2]

참가 물질

6

반응물 2

HCID 11356263Ethanone, 1-[3-methoxy-4-(methoxymethoxy)phenyl]-HCID 178418339Butyllithium

생성물 1

HCID 59643063HCID 59643063, 화합물

시약·촉매·용매 3

HCID 74505Methyltriphenyliphosphonium bromide촉매HCID 8028Tetrahydrofuran용매2회HCID 8058Hexane용매

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온도
-80 °C

실험 절차

A suspension of methyltriphenylphosphonium bromide (1.1 g, 3.09 mmol, 1.3 eq.) in 5 mL dry THF cooled to −80° C. was slowly treated with BuLi (1.94 mL of a 1.6 m solution in hexane, 1.3 eq.). To this yellow suspension a solution of 1-(3-methoxy-4-methoxymethoxy-phenyl)-ethanone (500 mg, 2.38 mmol, 1 eq.) in 5 mL dry THF was added and the reaction mixture was allowed to warm to r.t. where stirring was continued for 12 h. The suspension was filtered and the solvent was evaporated in vacuo. The crude product was purified using flash chromatography (silica gel, hexane/EtOAc 6:1) to yield the desired product as a color-less oil.

후처리

  1. temperatureto warm to r.t. where
  2. filtrationThe suspension was filtered
  3. customthe solvent was evaporated in vacuo
  4. customThe crude product was purified

출처 및 근거

ORD 기록
ord-4f8aca4ed01348d1be726ba7af91abfe
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07319101B2

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