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Toluene → HCID 89782323、化合物

HRID 1055915
ノート
印刷プレビュー

反応式

HRID 1055915 の反応式
C([Sn](CCCC)(CCCC)[C:6]([O:8]CC)=[CH2:7])CCC.Br[C:20]1[CH:21]=[CH:22][CH:23]=[C:24]2[C:29]=1[N:28]=[C:27]([C:30]([N:32]1[CH2:37][CH2:36][O:35][CH2:34][CH2:33]1)=[O:31])[CH:26]=[CH:25]2.C1(C)C=CC=CC=1.C(OC=C)=C>C1COCC1.Cl.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.CCOC(C)=O.CC(C)=O>[N:32]1([C:30]([C:27]2[CH:26]=[CH:25][C:24]3[C:29](=[C:20]([C:6](=[O:8])[CH3:7])[CH:21]=[CH:22][CH:23]=3)[N:28]=2)=[O:31])[CH2:37][CH2:36][O:35][CH2:34][CH2:33]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

10

反応物 4

HCID 1140TolueneHCID 8024Vinyl ether2 回HCID 619414Stannane, tributyl(1-ethoxyethenyl)-HCID 89781987HCID 89781987、化合物

生成物 1

HCID 89782323HCID 89782323、化合物収率 92.3%

試薬・触媒・溶媒 5

HCID 313Hydrochloric Acid触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 180Acetone溶媒2 回
HCID 8028Tetrahydrofuran溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

A mixture of Pd(PPh3)4 (18 mg, 0.016 mmol), tributyl(1-ethoxyvinyl)stannane (0.12 mL, 0.34 mmol), (8-bromoquinolin-2-yl)(morpholino)methanone (Example 167a; 100 mg, 0.31 mmol), and toluene (1.5 mL) were stirred in a sealed 5 mL glass microwave tube under argon at 100° C. for 63 h. Formation of both the vinyl ether (M+1=313.1) and the methyl ketone (M+1=285.0) were detected by LCMS. The mixture was concentrated under reduced pressure, and the residue was adsorbed onto silica gel. Chromatographic purification (silica gel, 10-70% EtOAc in hexanes) afforded a mixture of the vinyl ether and the methyl ketone as a colorless oil. The material was dissolved in THF (3 mL), the solution was cooled to 0° C., 2 drops of 1N HCl were added and the solution was stirred at 0° C. for 5 min. EtOAc (25 mL) was added to the reaction mixture and the solution was washed successively with 1N NaOH (5 mL), water (10 mL) and brine (10 mL). The combined aq. washes were extracted with 25% IPA in CHCl3, and all organic layers were then combined, dried over MgSO4, filtered, and concentrated in vacuo to give 1-(2-(morpholine-4-carbonyl)quinolin-8-yl)ethanone (81.4 mg, 0.286 mmol, 92% yield) as a white film: 1H NMR (400 MHz, DMSO-d6) δ ppm 8.62 (d, J=8.6 Hz, 1H), 8.18-8.24 (m, 1H), 7.95 (dd, J=7.1, 1.3 Hz, 1H), 7.72-7.83 (m, 2H), 3.72 (s, 4H), 3.56 (d, J=4.7 Hz, 4H), 2.79 (s, 3H). m/z (ESI, +ve ion) 285.0 (M+H)+.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customChromatographic purification (silica gel, 10-70% EtOAc in hexanes)
  3. customafforded
  4. temperaturethe solution was cooled to 0° C.
  5. stirringthe solution was stirred at 0° C. for 5 min
  6. washthe solution was washed successively with 1N NaOH (5 mL), water (10 mL) and brine (10 mL)
  7. extractionThe combined aq. washes were extracted with 25% IPA in CHCl3
  8. dry with materialdried over MgSO4
  9. filtrationfiltered
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-292c110d19e344fc9c28df614f502aee
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394297B2

反応ノート

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