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Toluene → 2-benzyl-5-(4-chlorophenyl)-4-methoxypyridazin-3(2H)-one

HRID 1865831
ノート
印刷プレビュー

反応式

HRID 1865831 の反応式
[CH2:1]([N:8]1[C:13](=[O:14])[C:12]([O:15][CH3:16])=[C:11](Cl)[CH:10]=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:18][C:19]1[CH:24]=[CH:23][C:22](B(O)O)=[CH:21][CH:20]=1.C1(C)C=CC=CC=1>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.C([O-])([O-])=O.[Na+].[Na+].CCO>[CH2:1]([N:8]1[C:13](=[O:14])[C:12]([O:15][CH3:16])=[C:11]([C:22]2[CH:23]=[CH:24][C:19]([Cl:18])=[CH:20][CH:21]=2)[CH:10]=[N:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=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

7

反応物 3

HCID 1140TolueneHCID 742994-Chlorophenylboronic acidHCID 135262132-Benzyl-5-chloro-4-methoxypyridazin-3(2H)-one

生成物 1

HCID 569275222-benzyl-5-(4-chlorophenyl)-4-methoxypyridazin-3(2H)-one収率 100,986.297%

試薬・触媒・溶媒 3

HCID 10340Sodium Carbonate触媒
HCID 178418397
HCID 178418397、化合物
触媒
HCID 702Ethanol溶媒

反応条件

温度
120 °C

実験手順

To a round bottom flask was added 2-benzyl-5-chloro-4-methoxypyridazin-3(2H)-one (25.1 gm, 0.1 mmol), 4-chlorophenyl boronic acid (17.215 gm, 0.11 mmol), Pd(PPh3)4(9.24 gm, 0.008 mmol), toluene (200 ml), EtOH (200 ml) and 2.0N Na2CO3 (200 ml, 0.4 mmol). The reaction was purged with argon for 10 min. The reaction was then heated to 120° C. and stirred at this temperature for 18 hrs. After this time, the reaction was cooled to rt, poured into a separatory funnel and the layers were separated. The aqueous layer was extracted with EtOAc (50 ml). The combined organic layers were washed with 1N NaOH (200 ml), water (200 ml) and saturated aqueous NaCl (200 ml). The organic layer was then slurried with MgSO4 to remove excess water, filtered and concentrated to give the crude product. The crude product was purified using an automated column chromatography system (ISCO, 330 gm silica gel) eluting with a gradient of 0-30% EtOAc/CH2Cl2 to give product 2-benzyl-5-(4-chlorophenyl)-4-methoxypyridazin-3(2H)-one (33 gm, 99% yield) as light yellow solid. HPLC retention time (method A) 3.740 min; LCMS (M+H)=327.2.

後処理

  1. customThe reaction was purged with argon for 10 min
  2. temperatureAfter this time, the reaction was cooled to rt
  3. additionpoured into a separatory funnel
  4. customthe layers were separated
  5. extractionThe aqueous layer was extracted with EtOAc (50 ml)
  6. washThe combined organic layers were washed with 1N NaOH (200 ml), water (200 ml) and saturated aqueous NaCl (200 ml)
  7. customto remove excess water
  8. filtrationfiltered
  9. concentrationconcentrated
  10. customto give the crude product
  11. customThe crude product was purified
  12. washeluting with a gradient of 0-30% EtOAc/CH2Cl2

出典と根拠

ORDレコード
ord-b382a18d96454e82bd33e4c83461ef2f
出典データセット
uspto-grants-2009_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07629342B2

反応ノート

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