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Triethylamine → (3R,4R)-2-(3,4-Dihydroxypyrrolidin-1-yl)-4-(3-fluorophenyl)-6-methoxyquinoline-3-carbonitrile

HRID 640727
ノート
印刷プレビュー

反応式

HRID 640727 の反応式
Cl[C:2]1[C:11]([C:12]#[N:13])=[C:10]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=2)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([O:21][CH3:22])[CH:8]=2)[N:3]=1.[OH:23][C@H:24]1[C@H:28]([OH:29])[CH2:27][NH:26][CH2:25]1.C(N(CC)CC)C>CC(O)C.CCOC(C)=O>[OH:23][C@H:24]1[C@H:28]([OH:29])[CH2:27][N:26]([C:2]2[C:11]([C:12]#[N:13])=[C:10]([C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([F:20])[CH:15]=3)[C:9]3[C:4](=[CH:5][CH:6]=[C:7]([O:21][CH3:22])[CH:8]=3)[N:3]=2)[CH2:25]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471Triethylamine2 回HCID 113703952-Chloro-4-(3-fluorophenyl)-6-methoxyquinoline-3-carbonitrileHCID 11499204(3R,4R)-pyrrolidine-3,4-diol2 回

生成物 1

HCID 11463095(3R,4R)-2-(3,4-Dihydroxypyrrolidin-1-yl)-4-(3-fluorophenyl)-6-methoxyquinoline-3-carbonitrile

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
150 °C

実験手順

A solution of 2-chloro-4-(3-fluorophenyl)-6-methoxyquinoline-3-carbonitrile (61.0 mg, 0.20 mmol), (3R,4R)-3,4-dihydroxypyrrolidine (43 mg, 0.42 mmol) and triethylamine (0.055 mL, 0.42 mmol) in 3 mL of 2-propanol was heated in a sealed tube at 120° C. for 3 days. The temperature was raised to 150° C. After 3 days, additional portions of (3R,4R)-3,4-dihydroxypyrrolidine (40 mg) and triethylamine (0.055 mL) were added. After a total of 11 days, the solution was cooled and diluted with EtOAc. The organic layer was washed with saturated NaHCO3 solution and brine, and dried over Na2SO4, filtered, and concentrated in vacuo. The crude residue was purified by recrystallization from EtOAc/hexane (40 mg, 54%). Proton NMR for the product was consistent with the titled compound. HRMS (ES) exact mass calculated for C21H19FN3O3 (M+M+): 380.1405. Found 380.1401.

後処理

  1. temperatureAfter a total of 11 days, the solution was cooled
  2. washThe organic layer was washed with saturated NaHCO3 solution and brine
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude residue was purified by recrystallization from EtOAc/hexane (40 mg, 54%)

出典と根拠

ORDレコード
ord-f19199f70c354cd69467086bdc40cb5d
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07692017B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート