Stannous Chloride → HCID 46944973、化合物

HRID 2370591ノート

反応式

HRID 2370591 の反応式
Cl[Sn]Cl.[CH3:4][C:5]1([CH3:45])[N:9]([CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][S:19][CH2:20][CH2:21][CH2:22][C:23]([F:29])([F:28])[C:24]([F:27])([F:26])[F:25])[C:8](=[O:30])[N:7]([C:31]2[CH:36]=[CH:35][C:34]([N+:37]([O-])=O)=[C:33]([C:40]([F:43])([F:42])[F:41])[CH:32]=2)[C:6]1=[O:44].C([O-])(O)=O.[Na+]>CCOC(C)=O>[NH2:37][C:34]1[CH:35]=[CH:36][C:31]([N:7]2[C:6](=[O:44])[C:5]([CH3:45])([CH3:4])[N:9]([CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][S:19][CH2:20][CH2:21][CH2:22][C:23]([F:28])([F:29])[C:24]([F:25])([F:26])[F:27])[C:8]2=[O:30])=[CH:32][C:33]=1[C:40]([F:43])([F:42])[F:41]

参加物

5

反応物 3

HCID 24479Stannous ChlorideHCID 516892Sodium BicarbonateHCID 46947722HCID 46947722、化合物

生成物 1

HCID 46944973HCID 46944973、化合物収率 84%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

SnCl2, 2H2O (3.84 g, 17 mmoles) is added to the compound of Example 1 (1.08 g, 1.7 mmole) dissolved in AcOEt (30 ml). The reaction mixture is heated under reflux until the starting compound disappears (5 h 30) and then cooled down using an ice bath. After dilution with AcOEt (30 ml), the mixture is poured onto a 1M aqueous solution of NaHCO3 (120 ml). The mixture is stirred for a few hours during which time a white precipitate forms. This precipitate is eliminated by filtration on celite. The filtrate is decanted and the organic solution is dried over Na2SO4, filtered and concentrated to dryness under vacuum. The expected compound is obtained in the form of a yellow oil with a yield of 84% (868 mg).

後処理

  1. temperatureThe reaction mixture is heated
  2. temperatureunder reflux until the starting compound
  3. custom(5 h 30)
  4. temperaturecooled down
  5. filtrationThis precipitate is eliminated by filtration on celite
  6. customThe filtrate is decanted
  7. dry with materialthe organic solution is dried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated to dryness under vacuum

出典と根拠

ORDレコード
ord-347556575c6949e7a3bfd32ce3f27429
出典データセット
uspto-grants-2014_04
特許番号
US08710091B2

反応ノート

読み込み中…