Acetonitrile → HCID 20064747, 화합물

HRID 359286노트

반응식

HRID 359286 반응식
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]

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 6363IsopropylamineHCID 91715Flurazole

생성물 1

HCID 20064747HCID 20064747, 화합물수율 62%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-11fb6164c4c545a89af5d250b561c05d
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05000775

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