Ethanol → HCID 22397820、化合物

HRID 1483919ノート

反応式

HRID 1483919 の反応式
Br[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([S:8]([C:11]([F:14])([F:13])[F:12])(=[O:10])=[O:9])[CH:3]=1.[N:15]1[CH:20]=[CH:19][C:18](B(O)O)=[CH:17][CH:16]=1.CCO.C([O-])([O-])=O.[Na+].[Na+]>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(Cl)Cl>[F:12][C:11]([F:14])([F:13])[S:8]([C:4]1[CH:3]=[C:2]([C:18]2[CH:19]=[CH:20][N:15]=[CH:16][CH:17]=2)[CH:7]=[CH:6][CH:5]=1)(=[O:10])=[O:9]

参加物

8

反応物 4

HCID 702EthanolHCID 10340Sodium CarbonateHCID 2734379(Pyridin-4-yl)boronic acidHCID 223978261-Bromo-3-((trifluoromethyl)sulfonyl)benzene

生成物 1

HCID 22397820HCID 22397820、化合物

試薬・触媒・溶媒 3

HCID 178418397HCID 178418397、化合物触媒HCID 1140Toluene溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
90 °C

実験手順

1-Bromo-3-trifluoromethylsulfonyl benzene (580 mg) and 4-pyridine-boronic acid (275 mg) was dissolved in toluene (5 ml) and abs EtOH (5 ml). To the mixture was then added Na2CO3 (424 mg) and Pd(PPh3)4 (119 mg) under an atmosphere of Argon. The resulting mixture was heated to 90° C. for 18 h. Then CH2Cl2 was added and the organic phase was washed with water and dried (MgSO4), filtered and evaporated to dryness. The residue was then used without any further purification. (MS m/z (rel. intensity, 70 eV) 287 (M+, 33), 218 (22), 154 (bp), 127 (56), 69 (27).

後処理

  1. washthe organic phase was washed with water
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customThe residue was then used without any further purification

出典と根拠

ORDレコード
ord-8a77c5eb498c43faa16ecd5c05705026
出典データセット
uspto-grants-2016_08
特許番号
USRE046117E1

反応ノート

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