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Water → HCID 69048427、化合物

HRID 733166
ノート
印刷プレビュー

反応式

HRID 733166 の反応式
C(=O)([O-])[O-].[K+].[K+].O.Cl[C:9]1[CH:14]=[C:13]([CH2:15][CH2:16][CH3:17])[N:12]=[C:11]([S:18]([CH3:21])(=[O:20])=[O:19])[N:10]=1.[CH:22]([C:25]1[CH:26]=[C:27](B(O)O)[CH:28]=[CH:29][CH:30]=1)([CH3:24])[CH3:23]>C(COC)OC.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>[CH:22]([C:25]1[CH:30]=[C:29]([C:9]2[CH:14]=[C:13]([CH2:15][CH2:16][CH3:17])[N:12]=[C:11]([S:18]([CH3:21])(=[O:20])=[O:19])[N:10]=2)[CH:28]=[CH:27][CH:26]=1)([CH3:24])[CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 27734783-Isopropylbenzeneboronic acidHCID 86619633HCID 86619633、化合物

生成物 1

HCID 69048427HCID 69048427、化合物収率 23.9%

試薬・触媒・溶媒 2

HCID 178418397
HCID 178418397、化合物
触媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

Potassium carbonate (0.850 g, 6 mmol), water (1 ml) and tetrakis(triphenylphosphine)palladium (0.695 g, 0.6 mmol) were successively added under a nitrogen atmosphere, to a mixture of 4-chloro-2-methanesulfonyl-6-propyl-pyrimidine (1.17 g, 5 mmol) and 3-isopropyl-phenylboronic acid (0.984 g, 6 mmol) in dimethoxyethane (40 mL). The mixture was refluxed for 18 hours then concentrated under reduced pressure. The residue was partitioned between ethyl acetate and water. The aqueous layer was extracted twice with ethyl acetate. The combined organic layers were dried over sodium sulphate, filtered and concentrated under reduced pressure. The residue was chromatographed over silica gel (eluent: Cyclohexane/Ethyl acetate 7/3) to afford a yellow oil which crystallised in pentane. After filtration, 4-(3-isopropyl-phenyl)-2-methanesulfonyl-6-propyl-pyrimidine (0.380 g) was obtained as an off white solid (mp=82° C.).

後処理

  1. temperatureThe mixture was refluxed for 18 hours
  2. concentrationthen concentrated under reduced pressure
  3. customThe residue was partitioned between ethyl acetate and water
  4. extractionThe aqueous layer was extracted twice with ethyl acetate
  5. dry with materialThe combined organic layers were dried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was chromatographed over silica gel (eluent: Cyclohexane/Ethyl acetate 7/3)
  9. customto afford a yellow oil which
  10. customcrystallised in pentane
  11. filtrationAfter filtration

出典と根拠

ORDレコード
ord-eb011ff728b74ea9baef984b3506d68c
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07589095B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート