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4-(Benzyloxy)-3-methoxybenzaldehyde → (E)-4-[3-Methoxy-4-(phenylmethoxy)phenyl]-3-buten-1-ol

HRID 1721961
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HRID 1721961 반응식
C([Li])CCC.[Br-].[OH:7][CH2:8][CH2:9][CH2:10][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[CH3:30][O:31][C:32]1[CH:33]=[C:34]([CH:37]=[CH:38][C:39]=1[O:40][CH2:41][C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1)[CH:35]=O>C1COCC1>[CH3:30][O:31][C:32]1[CH:33]=[C:34](/[CH:35]=[CH:10]/[CH2:9][CH2:8][OH:7])[CH:37]=[CH:38][C:39]=1[O:40][CH2:41][C:42]1[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1
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참가 물질

5

반응물 3

HCID 755064-(Benzyloxy)-3-methoxybenzaldehydeHCID 11025793(3-Hydroxypropyl)triphenylphosphonium bromideHCID 178418339Butyllithium

생성물 1

HCID 19862737(E)-4-[3-Methoxy-4-(phenylmethoxy)phenyl]-3-buten-1-ol수율 34%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

n-Butyllithium (1.55M in hexane, 194 ml) was added dropwise to a stirred suspension of (3-hydroxypropyl)triphenylphosphonium bromide (60.3 g) in dry THF (375 ml) cooled to 0° under nitrogen. The resulting blood-red solution was stirred at 0° for 15 min and then a solution of 3-methoxy-4-(phenylmethoxy)benzaldehyde (36.3 g) in dry THF (50 ml) was added dropwise over 15 min. The mixture was stirred at 0° for 30 min, allowed to warm up to room temperature, stirred for a further 2 h and then the reaction quenched by the addition of 2N hydrochloric acid (100 ml). The THF was removed in vacuo at 40°, the aqueous residue extracted with ethyl acetate (350 ml) and the organic layer washed with 2N HCl (200 ml). The aqueous phase was extracted with further ethyl acetate (150 ml), the organic layers combined, washed with 8% sodium bicarbonate solution (200 ml) and dried. Concentration afforded a product which was purified by FCC eluting with System B (1:2) yielding the title compound as a cream powder (14.5 g) m.p. 57°-61°

후처리

  1. temperaturecooled to 0° under nitrogen
  2. stirringThe mixture was stirred at 0° for 30 min
  3. stirringstirred for a further 2 h
  4. customthe reaction quenched by the addition of 2N hydrochloric acid (100 ml)
  5. customThe THF was removed in vacuo at 40°
  6. extractionthe aqueous residue extracted with ethyl acetate (350 ml)
  7. washthe organic layer washed with 2N HCl (200 ml)
  8. extractionThe aqueous phase was extracted with further ethyl acetate (150 ml)
  9. washwashed with 8% sodium bicarbonate solution (200 ml)
  10. customdried
  11. concentrationConcentration
  12. customafforded a product which
  13. customwas purified by FCC
  14. washeluting with System B (1:2)

출처 및 근거

ORD 기록
ord-aa63562e998247d29e2b740e6a9d1769
출처 데이터셋
uspto-grants-1989_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04853381

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