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Benzenamine, 3-(methylthio)- → HCID 11529322、化合物

HRID 1437739
ノート
印刷プレビュー

反応式

HRID 1437739 の反応式
[Cl:1][C:2]1[CH:7]=[C:6](I)[CH:5]=[C:4]([Cl:9])[N:3]=1.[CH3:10][S:11][C:12]1[CH:13]=[C:14]([CH:16]=[CH:17][CH:18]=1)[NH2:15].C1(P(C2C=CC=CC=2)CCCP(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1.ClCCl.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[Cl:1][C:2]1[CH:7]=[C:6]([NH:15][C:14]2[CH:16]=[CH:17][CH:18]=[C:12]([S:11][CH3:10])[CH:13]=2)[CH:5]=[C:4]([Cl:9])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 15693Benzenamine, 3-(methylthio)-HCID 812191,3-Bis(diphenylphosphino)propaneHCID 117373932,6-Dichloro-4-iodopyridineHCID 23676156Sodium t-butoxide

生成物 1

HCID 11529322HCID 11529322、化合物

試薬・触媒・溶媒 3

HCID 9811564
Bis(dibenzylideneacetone)palladium
触媒
HCID 1140Toluene溶媒
HCID 6344Dichloromethane溶媒

実験手順

To 2,6-dichloro-4-iodopyridine (1.3715 g, 5 mmol) dissolved in toluene (30 mL) were added 3-methylthioaniline (0.73 mL, 6 mmol), tris(dibenzylidene-acetone)dipalladium (90.6 mg, 0.1 mmol), 1,3-bis(diphenylphosphino)propane (80.0 mg, 0.2 mmol), and sodium-tert-butoxide (672.1 mg, 7 mmol). The resulting mixture was allowed to stir at reflux for 12-18 hours. The sample was diluted in dichloromethane and filtered through Celite™. The Celite™ was washed with dichloromethane and the filtrate was washed two times with water and one time with brine. The organic phase was dried over potassium carbonate and concentrated by rotary evaporation. The resulting sample (9) was dried for 12-18 hours under vacuum. The sample was used without purification.

後処理

  1. temperatureat reflux for 12-18 hours
  2. filtrationfiltered through Celite™
  3. washThe Celite™ was washed with dichloromethane
  4. washthe filtrate was washed two times with water and one time with brine
  5. dry with materialThe organic phase was dried over potassium carbonate
  6. concentrationconcentrated by rotary evaporation
  7. dry with materialThe resulting sample (9) was dried for 12-18 hours under vacuum
  8. customThe sample was used without purification

出典と根拠

ORDレコード
ord-49d992825ad2495da4b2436a5d76dd94
出典データセット
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07622486B2

反応ノート

読み込み中…

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