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Sodium Carbonate → HCID 10990505、化合物

HRID 1358967
ノート
印刷プレビュー

反応式

HRID 1358967 の反応式
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([Cl:9])=[CH:4][C:3]=1B(O)O.[NH2:13][C:14]1[C:19](Br)=[N:18][CH:17]=[C:16]([Cl:21])[N:15]=1.C(=O)([O-])[O-].[Na+].[Na+]>C(O)C.C1C=CC=CC=1>[NH2:13][C:14]1[C:19]([C:3]2[CH:4]=[C:5]([Cl:9])[CH:6]=[C:7]([Cl:8])[C:2]=2[Cl:1])=[N:18][CH:17]=[C:16]([Cl:21])[N:15]=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 3

HCID 10340Sodium CarbonateHCID 51065082,3,5-Trichlorophenylboronic acidHCID 179559912-Amino-3-bromo-6-chloropyrazine

生成物 1

HCID 10990505HCID 10990505、化合物

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 702Ethanol溶媒

実験手順

A solution of 2,3,5-trichlorobenzeneboronic acid (1.62 g, 7.18×10−3 mole) in absolute ethanol (2.05 ml) was added slowly to a mixture of 2-amino-3-bromo-6 chloropyrazine (1 g, 5.1×10−3 mole) and tetrakis(triphenylphospine)palladium(O) (0.334 g, 2.89×10−4 mole) in benzene (10.20 ml)/2M aqueous sodium carbonate (5.50 ml). The mixture was refluxed for 17 hrs. The cooled reaction mixture was evaporated in vacuo and then extracted with chloroform (50 ml). The chloroform layer was washed with water (2×30 ml), dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated down in vacuo. The residue was triturated with 40-60° C. petroleum ether, filtered and dried in vacuo. Yield 0.205 g (14%), M.p. 211-214° C.

後処理

  1. temperatureThe mixture was refluxed for 17 hrs
  2. customThe cooled reaction mixture
  3. customwas evaporated in vacuo
  4. extractionextracted with chloroform (50 ml)
  5. washThe chloroform layer was washed with water (2×30 ml)
  6. dry with materialdried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. customthe filtrate evaporated down in vacuo
  9. customThe residue was triturated with 40-60° C. petroleum ether
  10. filtrationfiltered
  11. customdried in vacuo

出典と根拠

ORDレコード
ord-4ce67c62932e43fb9291240c4ac1970a
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06599905B2

反応ノート

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