HCID 4415129、化合物 → HCID 67367547、化合物

HRID 383984ノート

反応式

HRID 383984 の反応式
[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

参加物

3

反応物 1

HCID 4415129HCID 4415129、化合物

生成物 1

HCID 67367547HCID 67367547、化合物収率 27.6%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
150 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-618f3b3c39a14629b3007f5e1508c08e
出典データセット
uspto-grants-2013_02
特許番号
US08367700B2

反応ノート

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