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Methyl Ethyl Ketone → HCID 20484885、化合物

HRID 647432
ノート
印刷プレビュー

反応式

HRID 647432 の反応式
Br[CH:2]([CH3:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[Cl:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[C:17]([F:20])[CH:18]=2)[CH:13]=[C:12]([N:21]([C:23]2[CH:28]=[CH:27][C:26]([OH:29])=[CH:25][CH:24]=2)[CH3:22])[N:11]=1.C(=O)([O-])[O-].[K+].[K+].C(C(C)=O)C>ClCCl>[Cl:9][C:10]1[C:19]2[C:14](=[CH:15][CH:16]=[C:17]([F:20])[CH:18]=2)[CH:13]=[C:12]([N:21]([C:23]2[CH:28]=[CH:27][C:26]([O:29][CH:2]([CH3:8])[C:3]([O:5][CH2:6][CH3:7])=[O:4])=[CH:25][CH:24]=2)[CH3:22])[N:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 79040Ethyl 2-bromopropionateHCID 133862374-[N-(1-chloro-7-fluoroisoquinolin-3-yl)-N-methylamino]phenol

生成物 1

HCID 20484885HCID 20484885、化合物収率 88.4%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

A mixture of ethyl 2-bromopropionate (1.12 g), 4-[N-(1-chloro-7-fluoroisoquinolin-3-yl)-N-methylamino]phenol (1.70 g), anhydrous potassium carbonate (0.86 g) and methyl ethyl ketone (20 ml) was heated under reflux for a period of 3 hours. The mixture was cooled, diluted with dichloromethane, washed with water and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure to give an oil which was purified by column chromatography over silica gel (eluant dichloromethane) to give ethyl 2-{4-[N-(1-chloro-7-fluoroisoquinolin-3-yl)-N-methylamino]phenoxy}propionate (2.00 g) as a yellow oil. The assigned structure was confirmed by proton magnetic spectroscopy and mass spectrometry. Proton magnetic resonance spectrum (CDCl3 ; δ in ppm): 1.29 (3H, t); 1.65 (3H, d); 3.47 (3H, s); 4.27 (2H, q); 4.75 (1H, q); 6.47 (1H, s) 6.85-7.20 (6H, m); 7.30 (1H, d).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for a period of 3 hours
  3. temperatureThe mixture was cooled
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was removed by distillation under reduced pressure
  7. customto give an oil which
  8. customwas purified by column chromatography over silica gel (eluant dichloromethane)

出典と根拠

ORDレコード
ord-a7bc75368ebb43ab8d622e1a4fb51688
出典データセット
uspto-grants-1983_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04409017

反応ノート

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