Acetonitrile → HCID 20064747、化合物

HRID 359286ノート

反応式

HRID 359286 の反応式
C(#N)C.[CH:4]([NH2:7])([CH3:6])[CH3:5].Cl[C:9]1[S:10][C:11]([C:18]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:19])=[C:12]([C:14]([F:17])([F:16])[F:15])[N:13]=1>C(OCC)C>[CH3:5][CH:4]([NH:7][C:9]1[S:10][C:11]([C:18]([O:20][CH2:21][C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)=[O:19])=[C:12]([C:14]([F:16])([F:15])[F:17])[N:13]=1)[CH3:6]

参加物

5

反応物 3

HCID 6342AcetonitrileHCID 6363IsopropylamineHCID 91715Flurazole

生成物 1

HCID 20064747HCID 20064747、化合物収率 62%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A reaction vessel was charged with 25 ml of acetonitrile, 2.94 g (49.8 mmol) of iso-propylamine, and 8 g (24.9 mmol) of benzyl 2-chloro-4-trifluoromethyl-5-thiazolecarboxylate (prepared as described in U.S. Pat. No. 4,199,506). The reaction mixture was heated at reflux for 16 hours. The mixture was then cooled to ambient temperature, diluted with ethyl ether, washed with large amounts of water, dried over magnesium sulfate, and concentrated under reduced pressure to yield 5.32 g of a gold oil. This oil was subjected - to Kugelrohr distillation (145°-155° C. @ 0.5 mm Hg) to yield 4.97 of a gold oil which was then triturated in hexane to yield 3.99 g of a yellow solid product (m.p.=49°-53° C.) identified in Table I.

後処理

  1. customprepared
  2. temperatureThe reaction mixture was heated
  3. temperatureat reflux for 16 hours
  4. washwashed with large amounts of water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-11fb6164c4c545a89af5d250b561c05d
出典データセット
uspto-grants-1991_03
特許番号
US05000775

反応ノート

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