HCID 4415129, 화합물 → HCID 67367547, 화합물

HRID 383984노트

반응식

HRID 383984 반응식
[F:1][C:2]1[CH:18]=[CH:17][C:5]([CH2:6][CH2:7][NH:8][C:9](=O)[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1>O>[F:1][C:2]1[CH:18]=[C:17]2[C:5]([CH2:6][CH2:7][N:8]=[C:9]2[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1

참가 물질

3

반응물 1

HCID 4415129HCID 4415129, 화합물

생성물 1

HCID 67367547HCID 67367547, 화합물수율 27.6%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

A mixture of 12.5 g (51.4 mmol) of N-(4-fluorophenethyl)benzamide and polyphosphoric acid (150 ml) was heated at 150° C. for 5 days. Then the hot solution was poured into water and the reaction was quenched by the addition of NaHCO3. It was extracted with DCM (3×300 ml). The combined organic phases were washed with brine (300 ml), dried over Na2SO4, filtered and concentrated to small volume under vacuum. 3.2 g of the crude product 7-fluoro-1-phenyl-3,4-dihydroisoquinoline were obtained as the residue, which was reacted further with no additional purification.

후처리

  1. customthe reaction was quenched by the addition of NaHCO3
  2. extractionIt was extracted with DCM (3×300 ml)
  3. washThe combined organic phases were washed with brine (300 ml)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated to small volume under vacuum

출처 및 근거

ORD 기록
ord-618f3b3c39a14629b3007f5e1508c08e
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367700B2

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